CN107036997A - Method and application using the preparation process of near infrared spectroscopy quick detection qizhi weitong granules - Google Patents
Method and application using the preparation process of near infrared spectroscopy quick detection qizhi weitong granules Download PDFInfo
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- CN107036997A CN107036997A CN201610997258.2A CN201610997258A CN107036997A CN 107036997 A CN107036997 A CN 107036997A CN 201610997258 A CN201610997258 A CN 201610997258A CN 107036997 A CN107036997 A CN 107036997A
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- qizhi weitong
- weitong granules
- near infrared
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- 239000009737 qizhiweitong Substances 0.000 title claims abstract description 240
- 238000001514 detection method Methods 0.000 title claims abstract description 106
- 238000002360 preparation method Methods 0.000 title claims abstract description 48
- 238000004497 NIR spectroscopy Methods 0.000 title claims abstract description 28
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- YKRGDOXKVOZESV-WRJNSLSBSA-N Paeoniflorin Chemical compound C([C@]12[C@H]3O[C@]4(O)C[C@](O3)([C@]1(C[C@@H]42)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)C)OC(=O)C1=CC=CC=C1 YKRGDOXKVOZESV-WRJNSLSBSA-N 0.000 claims description 103
- YKRGDOXKVOZESV-UHFFFAOYSA-N paeoniflorin Natural products O1C(C)(C2(CC34)OC5C(C(O)C(O)C(CO)O5)O)CC3(O)OC1C24COC(=O)C1=CC=CC=C1 YKRGDOXKVOZESV-UHFFFAOYSA-N 0.000 claims description 103
- 238000002329 infrared spectrum Methods 0.000 claims description 92
- 238000003556 assay Methods 0.000 claims description 57
- DFPMSGMNTNDNHN-ZPHOTFPESA-N naringin Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@H]1[C@H](OC=2C=C3O[C@@H](CC(=O)C3=C(O)C=2)C=2C=CC(O)=CC=2)O[C@H](CO)[C@@H](O)[C@@H]1O DFPMSGMNTNDNHN-ZPHOTFPESA-N 0.000 claims description 52
- ARGKVCXINMKCAZ-UZRWAPQLSA-N neohesperidin Chemical compound C1=C(O)C(OC)=CC=C1[C@H]1OC2=CC(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O[C@H]3[C@@H]([C@H](O)[C@@H](O)[C@H](C)O3)O)=CC(O)=C2C(=O)C1 ARGKVCXINMKCAZ-UZRWAPQLSA-N 0.000 claims description 48
- ARGKVCXINMKCAZ-UHFFFAOYSA-N neohesperidine Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(OC3C(C(O)C(O)C(CO)O3)OC3C(C(O)C(O)C(C)O3)O)=CC(O)=C2C(=O)C1 ARGKVCXINMKCAZ-UHFFFAOYSA-N 0.000 claims description 48
- 238000001228 spectrum Methods 0.000 claims description 47
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 18
- 239000003814 drug Substances 0.000 claims description 18
- 239000001606 7-[(2S,3R,4S,5S,6R)-4,5-dihydroxy-6-(hydroxymethyl)-3-[(2S,3R,4R,5R,6S)-3,4,5-trihydroxy-6-methyloxan-2-yl]oxyoxan-2-yl]oxy-5-hydroxy-2-(4-hydroxyphenyl)chroman-4-one Substances 0.000 claims description 15
- 229940052490 naringin Drugs 0.000 claims description 15
- 229930019673 naringin Natural products 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
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- QUQPHWDTPGMPEX-UTWYECKDSA-N aurantiamarin Natural products COc1ccc(cc1O)[C@H]1CC(=O)c2c(O)cc(O[C@@H]3O[C@H](CO[C@@H]4O[C@@H](C)[C@H](O)[C@@H](O)[C@H]4O)[C@@H](O)[C@H](O)[C@H]3O)cc2O1 QUQPHWDTPGMPEX-UTWYECKDSA-N 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 238000010986 on-line near-infrared spectroscopy Methods 0.000 abstract description 3
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- 239000001947 glycyrrhiza glabra rhizome/root Substances 0.000 description 2
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
It the present invention relates to the use of method and the application of the preparation process of near infrared spectroscopy quick detection qizhi weitong granules.The present invention establishes the preparation process reclaimed water extraction process of qizhi weitong granules, extracts volatile oil process and the on-line near infrared spectroscopy analysis method of extract solution concentration process, and it is applied to on-line checking, realize the automatic detection of the preparation process of qizhi weitong granules and the real-time estimate of each quality control index content；The model prediction accuracy set up is high, and the degree of accuracy is high, meets the requirement of quantitative analysis in actual production；This method is compared with traditional official method, on the basis of the degree of accuracy is ensured, analysis efficiency is substantially increased, quality that can be fast and efficiently to extraction process is monitored and controlled in real time, so as to advantageously ensure that the security of end product quality, stability and validity.
Description
Technical field
The invention belongs to drug tests, and in particular to utilize near infrared spectroscopy quick detection qizhi weitong granules
The method of preparation process and application.
Background technology
Qizhi weitong granules is made up of radix bupleuri, corydalis tuber, Fructus Aurantii, rhizoma cyperi, the root of herbaceous peony and the taste Chinese medicine of honey-fried licorice root 6, with easypro liver
Qi-regulating and the effect of stomach and alleviating pain, for the treatment of the diseases such as stagnation of QI due to depression of the liver, feeling of stuffiness in chest turgor, gastral cavity pain, by clinical for many years real
Trample, the fiest-tire medication as clinical treatment epigastric pain.But, the preparation process of qizhi weitong granules is complicated and cumbersome, real
The minor variations of various technological parameters are likely to directly affect the quality of final medicine in the production process of border.
Traditional Pharmaceutical Analysis technology typically uses offline analysis means, and decoction is gathered from extractor and concentration tank,
Analyzed in the lab by high performance liquid chromatography, gas-chromatography etc., the result after analysis is then fed back into production car
Between carry out production regulation and control.However, traditional analysis mode is due to inefficiency, production efficiency is not only leveraged, and be difficult
Reflect chemical change complicated in extraction process and concentration process and physical change.Promoting modernization of industry of Chinese materia medica development
In process, with the continuous improvement of China's drug production process automaticity, in order to ensure the homogeneity of tcm product quality
And stability, the fast mass analysis method and online measuring technique of Study of Traditional Chinese Medicine pharmacy procedure, produced for improving China's Chinese medicine
Industry modernization level is significant.
Near infrared spectrum (NearInfraredSpectrumInstrument, NIRS) is one developed rapidly in recent years
Effectively easy analysis method is planted, by being combined with optical fiber and computer technology, NIR measurement signals can carry out long distance
From transmission and analysis.Near infrared light is a kind of electromagnetic wave, between visible ray (Vis) and in electromagnetic radiation between infrared (MIR)
Ripple, wavelength is in 780-2526nm, and near-infrared spectrum analysis has that free from environmental pollution, sampling without damage, analyze speed be fast, operation letter
List, real-time online, overall merit, the degree of accuracy are high, analysis object extensively, without consumables associated therewith and the features such as maintenance cost.It is near red
External spectrum area is consistent with sum of fundamental frequencies that hydric group in organic molecule (O-H, N-H, C-H) vibrates and the uptake zone of frequency multiplication at different levels, leads to
The near infrared spectrum of sample is over-scanned, the characteristic information of organic molecule hydric group in sample can be obtained, near infrared light is utilized
The maximum feature of spectral technology analysis sample is quick, lossless, in situ online etc., and therefore, the technology is increasingly by researcher
Favor.At present, near-infrared spectrum technique obtains relatively successfully application in fields such as medicine, oil, food industry.
Therefore, a kind of method for the preparation process that can rapidly, comprehensively detect qizhi weitong granules is set up, to the stagnation of the circulation of vital energy
The production in enormous quantities and overall quality control of stomachache particle are significant.
The content of the invention
Therefore, the present invention provides a kind of side of the preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules
Method and application.
In order to solve the above technical problems, the present invention is achieved through the following technical solutions：
The present invention provides a kind of method of the preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules,
The detection of water extraction process including following qizhi weitong granules and/or the extraction volatile oil mistake of qizhi weitong granules
The detection of journey and/or the detection of the extract solution concentration process of qizhi weitong granules：
A, the water extraction process of qizhi weitong granules detection
The step of assay and/or determination of solid content including following Paeoniflorin:
A, the assay of Paeoniflorin comprise the following steps：
(1) aqueous extract of the qizhi weitong granules of known paeoniflorin content is taken, it is standby；
(2) aqueous extract of the qizhi weitong granules is subjected near infrared spectrum scanning, gathers the energy-stagnation stomachache
The near infrared spectrum of the aqueous extract of grain；
(3) 5448.8~6102.7cm is chosen-1With 6201~6501cm-1Spectral information under characteristic wave bands, applied chemistry
The paeoniflorin content of meterological software and the aqueous extract of the qizhi weitong granules of the known paeoniflorin content is associated, and is adopted
The quantitative calibration model set up with PLS between near infrared spectrum and standard content；
(4) near infrared light is carried out to the aqueous extract sample of unknown qizhi weitong granules according to the method for the step (2)
Spectrum scanning, and choose 5448.8~6102.7cm-1With 6201~6501cm-1Spectral information under characteristic wave bands, imports what is set up
Quantitative calibration model obtains the paeoniflorin content value of the aqueous extract sample of the unknown qizhi weitong granules；
B, determination of solid content comprise the following steps：
(1) aqueous extract of the qizhi weitong granules of known solid content is taken, it is standby；
(2) aqueous extract of the qizhi weitong granules is subjected near infrared spectrum scanning, gathers the energy-stagnation stomachache
The near infrared spectrum of the aqueous extract of grain；
(3) 6201~5701cm is chosen-1With 7170~7300cm-1Spectral information under characteristic wave bands, applied chemistry metering
The solid content for learning software and the aqueous extract of the qizhi weitong granules of the known solid content is associated, using offset minimum binary
The quantitative calibration model that method is set up between near infrared spectrum and standard content；
(4) near infrared light is carried out to the aqueous extract sample of unknown qizhi weitong granules according to the method for the step (2)
Spectrum scanning, and choose 6201~5701cm-1With 7170~7300cm-1Spectral information under characteristic wave bands, imports quantifying for foundation
Calibrating patterns obtain the solid content value of the aqueous extract sample of the unknown qizhi weitong granules；
B, the extraction volatile oil process of qizhi weitong granules detection
The step of assay and/or determination of solid content of assay, neohesperidin including following aurantiin:
A, the assay of aurantiin comprise the following steps：
(1) extract solution of the extraction volatile oil process of the qizhi weitong granules of known naringin content is taken, it is standby；
(2) extract solution of the extraction volatile oil process of the qizhi weitong granules is subjected near infrared spectrum scanning, collection
The near infrared spectrum of the extract solution of the extraction volatile oil process of the qizhi weitong granules；
(3) 5500~6100cm is chosen-1Spectral information under characteristic wave bands, Applied Chemometrics software with it is described known
The naringin content of the extract solution of the extraction volatile oil process of the qizhi weitong granules of naringin content is associated, using partially most
The quantitative calibration model that small square law is set up between near infrared spectrum and standard content；
(4) according to the step (2) method to unknown qizhi weitong granules extraction volatile oil process extract solution sample
Product carry out near infrared spectrum scanning, and choose 5500~6100cm-1Spectral information under characteristic wave bands, imports the quantitative school set up
Quasi-mode type obtains the naringin content value of the extract solution sample of the extraction volatile oil process of the unknown qizhi weitong granules；
B, the assay of neohesperidin comprise the following steps：
(1) extract solution of the extraction volatile oil process of the qizhi weitong granules of known neohesperidin content is taken, it is standby；
(2) extract solution of the extraction volatile oil process of the qizhi weitong granules is subjected near infrared spectrum scanning, collection
The near infrared spectrum of the extract solution of the extraction volatile oil process of the qizhi weitong granules；
(3) 7170~7270cm is chosen-1With 5500~6100cm-1Spectral information under characteristic wave bands, applied chemistry metering
Learn the neohesperidin of software and the extract solution of the extraction volatile oil process of the qizhi weitong granules of the known neohesperidin content
Content is associated, the quantitative calibration model set up using PLS between near infrared spectrum and standard content；
(4) according to the step (2) method to unknown qizhi weitong granules extraction volatile oil process extract solution sample
Product carry out near infrared spectrum scanning, and choose 7170~7270cm-1With 5500~6100cm-1Spectral information under characteristic wave bands,
Import the extract solution sample of the extraction volatile oil process for the quantitative calibration model acquisition unknown qizhi weitong granules set up
Neohesperidin content value；
C, determination of solid content comprise the following steps：
(1) extract solution of the extraction volatile oil process of the qizhi weitong granules of known solid content is taken, it is standby；
(2) extract solution of the extraction volatile oil process of the qizhi weitong granules is subjected near infrared spectrum scanning, collection
The near infrared spectrum of the extract solution of the extraction volatile oil process of the qizhi weitong granules；
(3) 5600~6000cm is chosen-1Spectral information under characteristic wave bands, Applied Chemometrics software with it is described known
The solid content of the extract solution of the extraction volatile oil process of the qizhi weitong granules of solid content is associated, using PLS
The quantitative calibration model set up between near infrared spectrum and standard content；
(4) according to the step (2) method to unknown qizhi weitong granules extraction volatile oil process extract solution sample
Product carry out near infrared spectrum scanning, and choose 5600~6000cm-1Spectral information under characteristic wave bands, imports the quantitative school set up
Quasi-mode type obtains the solid content value of the extract solution sample of the extraction volatile oil process of the unknown qizhi weitong granules；
C, the extract solution concentration process of qizhi weitong granules detection
The step of assay, relative density and/or determination of solid content including following Paeoniflorin:
A, the assay of Paeoniflorin comprise the following steps：
(1) concentrated extracting solution of the qizhi weitong granules of known paeoniflorin content is taken, it is standby；
(2) concentrated extracting solution of the qizhi weitong granules is subjected near infrared spectrum scanning, gathers the energy-stagnation stomachache
The near infrared spectrum of the concentrated extracting solution of particle；
(3) 5449.8~6101.7cm is chosen-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands, should
Entered with the paeoniflorin content of chemo metric software and the concentrated extracting solution of the qizhi weitong granules of the known paeoniflorin content
Row association, the quantitative calibration model set up using PLS between near infrared spectrum and standard content；
(4) near-infrared is carried out to the concentrated extracting solution sample of unknown qizhi weitong granules according to the method for the step (2)
Spectral scan, and choose 5449.8~6101.7cm-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands, leads
Enter the paeoniflorin content value of the concentrated extracting solution sample of the quantitative calibration model acquisition unknown qizhi weitong granules of foundation；
B, relative density determination comprise the following steps：
(1) concentrated extracting solution of the qizhi weitong granules of known relative density is taken, it is standby；
(2) concentrated extracting solution of the qizhi weitong granules is subjected near infrared spectrum scanning, gathers the energy-stagnation stomachache
The near infrared spectrum of the concentrated extracting solution of particle；
(3) 5469.13~7143.04cm is chosen-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands,
The relative density of Applied Chemometrics software and the concentrated extracting solution of the qizhi weitong granules of the known relative density is carried out
Association, the quantitative calibration model set up using PLS between near infrared spectrum and standard content；
(4) near-infrared is carried out to the concentrated extracting solution sample of unknown qizhi weitong granules according to the method for the step (2)
Spectral scan, and choose 5469.13~7143.04cm-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands,
Import the relative density values that the quantitative calibration model set up obtains the concentrated extracting solution sample of the unknown qizhi weitong granules；
C, determination of solid content comprise the following steps：
(1) concentrated extracting solution of the qizhi weitong granules of known solid content is taken, it is standby；
(2) concentrated extracting solution of the qizhi weitong granules is subjected near infrared spectrum scanning, gathers the energy-stagnation stomachache
The near infrared spectrum of the concentrated extracting solution of particle；
(3) 5469.13~7143.04cm is chosen-1Spectral information under characteristic wave bands, Applied Chemometrics software and institute
The solid content for stating the concentrated extracting solution of the qizhi weitong granules of known solid content is associated, and sets up near using PLS
Quantitative calibration model between infrared spectrum and standard content；
(4) near-infrared is carried out to the concentrated extracting solution sample of unknown qizhi weitong granules according to the method for the step (2)
Spectral scan, and choose 5469.13~7143.04cm-1Spectral information under characteristic wave bands, imports the quantitative calibration model set up
Obtain the solid content value of the concentrated extracting solution sample of the unknown qizhi weitong granules.
Preferably, the side of the preparation process of above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules of the invention
Method,
The step of assay of Paeoniflorin in the detection of the water extraction process of the qizhi weitong granules (2) neutralization/
Or in the step of determination of solid content (2), carried out using static spectrum acquisition method the qizhi weitong granules aqueous extract it is near
Infrared spectrum is gathered, and actual conditions is：Spectral acquisition times are at intervals of 10min, using air as reference, and scanning times are 32 times,
Resolution ratio is 8cm-1, scanning optical spectrum scope is 4000~10000cm-1；
The step of assay of aurantiin in the detection of the extraction volatile oil process of the qizhi weitong granules (2)
In, the assay of neohesperidin the step of (2) in and/or the step of determination of solid content in (2), using static spectrum acquisition method
The near infrared spectra collection of the extraction volatile oil process of the qizhi weitong granules is carried out, actual conditions is：Spectral acquisition times
At intervals of 10min, using air as reference, scanning times are 32 times, and resolution ratio is 8cm-1, scanning optical spectrum scope be 4000~
10000cm-1；
In the step of assay of Paeoniflorin in the detection of the extract solution concentration process of the qizhi weitong granules (2)
And/or in the step of determination of solid content (2), the concentrated extracting solution of the qizhi weitong granules is carried out using static spectrum acquisition method
Near infrared spectra collection, actual conditions is：Spectral acquisition times are at intervals of 10min, using air as reference, and scanning times are 32
Secondary, resolution ratio is 8cm-1, scanning optical spectrum scope is 4000~10000cm-1。
It is further preferred that the preparation process of above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules of the invention
Method,
The step of assay of Paeoniflorin in the detection of the water extraction process of the qizhi weitong granules (2) neutralization/
Or in the step of determination of solid content (2), in addition to First derivative spectrograply and Norris are used to the near infrared spectrum collected
The step of derivative smoothing filter method is pre-processed；
In the step of assay of aurantiin in the detection of the extraction volatile oil process of the qizhi weitong granules (2)
And/or neohesperidin assay the step of (2) in, in addition to first derivative is used to the near infrared spectrum collected
The step of method and Norris derivative smoothing filter methods are pre-processed；
The qizhi weitong granules extraction volatile oil process detection in determination of solid content the step of (2) in, also wrap
Include the step of being pre-processed to the near infrared spectrum collected using First derivative spectrograply and S-G smothing filtering methods；
The step of assay of Paeoniflorin in the detection of the extract solution concentration process of the qizhi weitong granules (2)
In, in addition to the near infrared spectrum collected is located in advance using second derivative method and Norris derivative smoothings filter method
The step of reason；
It is in the step of relative density in the detection of the extract solution concentration process of the qizhi weitong granules (2) and/or solid
In the step of assay (2), in addition to First derivative spectrograply and Norris derivatives are used to the near infrared spectrum collected
The step of smothing filtering method is pre-processed.
The bulk drug composition and preparation method of qizhi weitong granules of the present invention are with reference to Chinese patent literature CN1712048A.
It is further preferred that the preparation process of above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules of the invention
Method,
The bulk drug of the qizhi weitong granules is constituted：
The parts by weight of radix bupleuri 30~100, the parts by weight of radix glycyrrhizae 15~60, the parts by weight of rhizoma cyperi 35~120, the weight of corydalis tuber 35~120
Measure part, the parts by weight of the root of herbaceous peony 40~150, the parts by weight of Fructus Aurantii 35~120.
It is further preferred that the preparation process of above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules of the invention
Method,
The preparation method of the qizhi weitong granules comprises the following steps：
(3) Fructus Aurantii and rhizoma cyperi of selected parts by weight are taken, volatile oil is extracted, decoction is standby, and the dregs of a decoction are discarded；
(4) radix bupleuri, radix glycyrrhizae, corydalis tuber and the root of herbaceous peony of selected parts by weight are taken, is added water to cook 2 times, the 1st decoction 0.5~4 is small
When, the 2nd decoction 0.5~3 hour；
(3) combining step (1) and the decocting liquid of step (2), filtering, filtrate be concentrated into relative density for 1.10~1.30 it is clear
Cream；
(4) particle is made in qinghuo reagent, plus auxiliary material, mixing, dries, and sprays into volatile oil, produces granule.
It is further preferred that the preparation process of above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules of the invention
Method,
The step of assay of Paeoniflorin in the detection of the water extraction process of the qizhi weitong granules (3) neutralization/
Or in the step of determination of solid content (3), in addition to the step evaluated the estimated performance of the quantitative calibration model of foundation
Suddenly, the evaluation index includes coefficient R, calibration set mean square deviation RMSEC, verifies that collection root mean square RMSEP, cross validation are square
Root RMSECV and prediction relative deviation RSEP, when R values closer to 1, RMSEC and RMSEP values it is smaller and closer to when, evaluation mould
Type stability is better, prediction precision is higher, then disclosure satisfy that the precision of prediction requirement of qizhi weitong granules Direct Analysis；Instead
It, then do not apply to；
The step of assay of aurantiin in the detection of the extraction volatile oil process of the qizhi weitong granules (3)
In, the assay of neohesperidin the step of (3) in and/or the step of determination of solid content in (3), in addition to described in foundation
The step of estimated performance of quantitative calibration model is evaluated, the evaluation index includes coefficient R, calibration set mean square deviation
RMSEC, checking collection root mean square RMSEP, cross validation root mean square RMSECV and prediction relative deviation RSEP, when R values closer to
1, RMSEC and RMSEP values it is smaller and closer to when, evaluation model stability is better, prediction precision is higher, then disclosure satisfy that gas
The precision of prediction requirement of indigestion pain particle Direct Analysis；Conversely, not applying to then；
The step of assay of Paeoniflorin in the detection of the extract solution concentration process of the qizhi weitong granules (3)
In, relative density determination the step of (3) in and/or the step of determination of solid content in (3), in addition to the quantitative school of foundation
The step of estimated performance of quasi-mode type is evaluated, the evaluation index includes coefficient R, calibration set mean square deviation RMSEC, tested
Card collection root mean square RMSEP, cross validation root mean square RMSECV and prediction relative deviation RSEP, when R values closer to 1, RMSEC with
RMSEP values it is smaller and closer to when, evaluation model stability is better, prediction precision is higher, then disclosure satisfy that energy-stagnation stomachache
The precision of prediction requirement of grain Direct Analysis；Conversely, not applying to then.
It is further preferred that the preparation process of above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules of the invention
Method,
The step of assay of Paeoniflorin in the detection of the water extraction process of the qizhi weitong granules (1) neutralization/
Or the Paeoniflorin in the detection of the extract solution concentration process of the qizhi weitong granules assay the step of (1) in, use
The paeoniflorin content of known paeoniflorin content qizhi weitong granules is used as standard content described in high effective liquid chromatography for measuring；
In the step of determination of solid content in the detection of the water extraction process of the qizhi weitong granules (3), the stagnation of the circulation of vital energy
Have a stomachache particle extraction volatile oil process detection in determination of solid content the step of (3) in and/or the qizhi weitong granules
Extract solution concentration process detection in determination of solid content the step of (3) in, the known solid content is determined using oven drying method
The solid content of qizhi weitong granules is used as standard content；
The step of assay of aurantiin in the detection of the extraction volatile oil process of the qizhi weitong granules (3)
In, the naringin content using known naringin content qizhi weitong granules described in high effective liquid chromatography for measuring contains as standard
Amount；
The step of assay of neohesperidin in the detection of the extraction volatile oil process of the qizhi weitong granules (3)
In, mark is used as using the neohesperidin content of known neohesperidin content qizhi weitong granules described in high effective liquid chromatography for measuring
Quasi- content.
It is further preferred that the preparation process of above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules of the invention
Method,
The paeoniflorin content of known paeoniflorin content qizhi weitong granules described in the use high effective liquid chromatography for measuring
Concretely comprise the following steps：
(1) concentrated extracting solution 4 of 4~6mL of aqueous extract or described qizhi weitong granuleses of the qizhi weitong granules is taken
~6mL, 8~12min is centrifuged under the conditions of rotating speed 12000-14000r/min, supernatant is taken, is used as need testing solution；
(2) precision weighs 1-3mg Paeoniflorin reference substances and is placed in 20mL measuring bottles, plus methanol be made every mL containing 0.05~
0.15mg solution, shakes up, and is used as reference substance solution；
(3) chromatographic condition：Using 4.6 × 250mm, 5 μm of Agilent Zorbax SB-C18 as chromatographic column, with 0.1% phosphorus
Aqueous acid is mobile phase A, according to following program carry out gradient elution by Mobile phase B of acetonitrile：0-13min, A：B is 85%：
15%；13-15min, A：B is 85%：15% → 10%：90%；15-19min, A：B is 10%：90%；19-25min, A：B
For 10%：90% → 0%：100%；25-30min, A：B is 0%：100% → 85%：15%；Flow velocity 1.0mL/min, column temperature
30 DEG C, Detection wavelength 230nm；
(4) it is accurate to draw the need testing solution and each 5 μ L of reference substance solution, liquid chromatograph is injected, is determined；
Using the tool of the naringin content of known naringin content qizhi weitong granules described in high effective liquid chromatography for measuring
Body step is：
(1) 4~6mL of extract solution of the extraction volatile oil process of the qizhi weitong granules is taken, in rotating speed 12000-
8~12min is centrifuged under the conditions of 14000r/min, supernatant is taken, is used as need testing solution；
(2) precision weighs 1-3mg aurantiin reference substances and is placed in 20mL measuring bottles, plus methanol be made every mL containing 0.05~
0.15mg solution, shakes up, and is used as reference substance solution；
(3) chromatographic condition：Using 4.6 × 250mm, 5 μm of Agilent Zorbax SB-C18 as chromatographic column, with 0.1% phosphorus
Aqueous acid is mobile phase A, according to following program carry out gradient elution by Mobile phase B of acetonitrile：0-18min, A：B is 80%：
20%；18-21min, A：B is 80%：20% → 10%：90%；21-25min, A：B is 10%：90%；21-30min, A：B
For 10%：90% → 0%：100%；30-35min, A：B is 0%：100% → 80%：20%；Flow velocity 1.0mL/min, column temperature
30 DEG C, Detection wavelength 283nm；
(4) it is accurate to draw the need testing solution and each 5 μ L of reference substance solution, liquid chromatograph is injected, is determined；
Using the neohesperidin content of known neohesperidin content qizhi weitong granules described in high effective liquid chromatography for measuring
Concretely comprise the following steps：
(1) 4~6mL of extract solution of the extraction volatile oil process of the qizhi weitong granules is taken, in rotating speed 12000-
8~12min is centrifuged under the conditions of 14000r/min, supernatant is taken, is used as need testing solution；
(2) precision weighs 1-3mg neohesperidin reference substances and is placed in 20mL measuring bottles, plus methanol be made every mL containing 0.05~
0.15mg solution, shakes up, and is used as reference substance solution；
(3) chromatographic condition：Using 4.6 × 250mm, 5 μm of Agilent Zorbax SB-C18 as chromatographic column, with 0.1% phosphorus
Aqueous acid is mobile phase A, according to following program carry out gradient elution by Mobile phase B of acetonitrile：0-18min, A：B is 80%：
20%；18-21min, A：B is 80%：20% → 10%：90%；21-25min, A：B is 10%：90%；21-30min, A：B
For 10%：90% → 0%：100%；30-35min, A：B is 0%：100% → 80%：20%；Flow velocity 1.0mL/min, column temperature
30 DEG C, Detection wavelength 283nm；
(4) it is accurate to draw the need testing solution and each 5 μ L of reference substance solution, liquid chromatograph is injected, is determined；
The use oven drying method determines concretely comprising the following steps for the solid content of the known solid content qizhi weitong granules：
The extraction of qizhi weitong granules described in the aqueous extract or 4~6mL of qizhi weitong granules described in 4~6mL is taken to volatilize
The concentrated extracting solution of qizhi weitong granules described in the extract solution or 4~6mL of oily process as drying to constant weight measuring cup, in
105 DEG C of 5~7h of drying, move to 20~40min of cooling in drier, weigh；Dried 0.5~1.5 hour at 105 DEG C, it is cold
But, weigh；Untill double difference of weighing is no more than 5mg, solid content is calculated.
The method that the present invention also provides the preparation process of above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules
Purposes in qizhi weitong granules quality testing and control.
Compared with prior art, above-mentioned technical proposal of the invention has advantages below：
(1) method of the preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules of the present invention, will
Near infrared spectroscopy is applied in the quality quick detection of the preparation process of qizhi weitong granules, for water extraction process, is extracted
Volatile oil process and extract solution concentration process determine quality control index respectively, can be to each preparation process (water of qizhi weitong granules
Extraction process, extraction volatile oil process and extract solution concentration process) quick measure, realize the preparation to qizhi weitong granules
Journey quickly, comprehensively detection, and have the advantages that simple to operate, accuracy is high, accuracy is high, can quickly judge stagnation of the circulation of vital energy stomach
Whether the preparation process (water extraction process, extraction volatile oil process and extract solution concentration process) of pain particle is qualified, shortens detection
Time, production cost is saved, improve production efficiency and economic benefit, it is ensured that qizhi weitong granules quality is safely, effectively；
(2) method of the preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules of the present invention, leads to
Cross each in the preparation process (water extraction process, extraction volatile oil process and extract solution concentration process) of selection qizhi weitong granules
Spectral band in the near infrared spectrum of quality control index, extracts effective characteristic spectrum wave band, this feature spectral band with according to
Each quality control index that existing conventional method is determined has good correlation, can effective monitoring qizhi weitong granules preparation process
Whether (water extraction process, extraction volatile oil process and extract solution concentration process) be qualified；
(3) method of the preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules of the present invention, pin
Each quality control index in preparation process (water extraction process, extraction volatile oil process and extract solution concentration process) is separately optimized
The preprocess method of near-infrared original spectrum, with filter information, reduces noise, improves this method detection qizhi weitong granules
The accuracy and accuracy of preparation process；
(4) present invention establishes the preparation process reclaimed water extraction process of qizhi weitong granules, extracts volatile oil process and carry
The on-line near infrared spectroscopy analysis method of liquid concentration process is taken, and is applied to on-line checking, qizhi weitong granules is realized
Preparation process automatic detection and the real-time estimate of each quality control index content；The model prediction accuracy set up is high, accurately
Degree is high, meets the requirement of quantitative analysis in actual production；This method is ensureing the basis of the degree of accuracy compared with traditional official method
On, analysis efficiency is substantially increased, quality that can be fast and efficiently to extraction process is monitored and controlled in real time, so that
Advantageously ensure that the security, stability and validity of end product quality.
Brief description of the drawings
In order that present disclosure is more likely to be clearly understood, specific embodiment and combination below according to the present invention
Accompanying drawing, the present invention is further detailed explanation, wherein：
Fig. 1 is the original atlas of near infrared spectra of the water extraction process of the qizhi weitong granules in embodiment 1；
Fig. 2 is the HPLC chromatogram of the Paeoniflorin reference substance in embodiment 1；
Fig. 3 is the HPLC chromatogram of the Paeoniflorin sample in embodiment 1；
Fig. 4 is that the near-infrared predicted value of the Paeoniflorin calibration set sample in embodiment 1 is related to efficient liquid phase measured value
Graph of a relation；
Fig. 5 is the near-infrared predicted value and the dependency relation figure of measured value of the solid content calibration set sample in embodiment 1；
Fig. 6 is that the Paeoniflorin in embodiment 1 verifies that the near-infrared predicted value of collection sample is related to efficient liquid phase measured value
Graph of a relation；
Fig. 7 is that the solid content checking in embodiment 1 collects the near-infrared predicted value of sample and the dependency relation figure of measured value；
Fig. 8 is the change in concentration that water extraction process one in embodiment 1 decocts liquid chromatogram measuring and model prediction Paeoniflorin
Compares figure；
Fig. 9 is that the water extraction process one in embodiment 1 decocts determination of solid content and model prediction solid content change compares figure；
Figure 10 is that the water extraction process two of the qizhi weitong granules in embodiment 1 decocts liquid chromatogram measuring and model prediction Chinese herbaceous peony
The change in concentration compares figure of medicine glycosides；
Figure 11 is that the water extraction process two of the qizhi weitong granules in embodiment 1 is decocted determination of solid content and contained admittedly with model prediction
Amount change compares figure；
Figure 12 is the original near infrared spectrum of the extraction volatile oil process of the qizhi weitong granules in embodiment 2；
Figure 13 is that the near-infrared predicted value of the aurantiin calibration set sample in embodiment 2 is related to efficient liquid phase measured value
Graph of a relation；
Figure 14 is the phase of the near-infrared predicted value and efficient liquid phase measured value of the neohesperidin calibration set sample in embodiment 2
Close graph of a relation；
Figure 15 is the near-infrared predicted value and the dependency relation figure of measured value of the solid content calibration set sample in embodiment 2；
Figure 16 is that the aurantiin checking in embodiment 2 collects the near-infrared predicted value of sample and the dependency relation of HPLC measured values
Figure；
Figure 17 is that the neohesperidin in embodiment 2 verifies the near-infrared predicted value of collection sample pass related to HPLC measured values
System's figure；
Figure 18 is that the solid content checking in embodiment 2 collects the near-infrared predicted value of sample and the dependency relation figure of measured value；
Figure 19 is that the liquid chromatogram measuring of extraction volatile oil process in embodiment 2 becomes with the concentration of model prediction aurantiin
Change compares figure；
Figure 20 is the concentration of the liquid chromatogram measuring and model prediction neohesperidin of the extraction volatile oil process in embodiment 2
Change compares figure；
Figure 21 is that the determination of solid content of the extraction volatile oil process in embodiment 2 is compareed with the change of model prediction solid content
Figure；
Figure 22 is the original near infrared spectrum of the extract solution concentration process of the qizhi weitong granules in embodiment 3；
Figure 23 is the Paeoniflorin reference substance chromatogram in embodiment 3；
Figure 24 is the Paeoniflorin sample chromatogram figure in embodiment 3；
Figure 25 is that the near-infrared predicted value of the Paeoniflorin calibration set sample in embodiment 3 is related to efficient liquid phase measured value
Graph of a relation；
Figure 26 is the near-infrared predicted value and the dependency relation of measured value of the relative density calibration set sample in embodiment 3
Figure；
Figure 27 is the near-infrared predicted value and the dependency relation figure of measured value of the solid content calibration set sample in embodiment 3；
Figure 28 is that the Paeoniflorin in embodiment 3 verifies that the near-infrared predicted value of collection sample is related to efficient liquid phase measured value
Graph of a relation；
Figure 29 is that the relative density checking in embodiment 3 collects the near-infrared predicted value of sample and the dependency relation of measured value
Figure；
Figure 30 is that the solid content checking in embodiment 3 collects the near-infrared predicted value of sample and the dependency relation figure of measured value；
Figure 31 is the change in concentration of the extract solution concentration process liquid chromatogram measuring in embodiment 3 and model prediction Paeoniflorin
Compares figure；
Figure 32 is that extract solution concentration process relative density determination and the concentration of model prediction relative density in embodiment 3 become
Change compares figure；
Figure 33 is the change in concentration pair of the extract solution concentration process determination of solid content in embodiment 3 and model prediction solid content
According to figure.
Embodiment
Embodiment 1Near-infrared spectrum technique is used for the research of qizhi weitong granules preparation process reclaimed water extraction process
1. instrument and reagent
1.1 main Chinese medicinal materials and reagent
Radix bupleuri, the root of herbaceous peony, honey-fried licorice root, corydalis tuber (processing) (Liaoning Huarun Benxi Third Pharmaceutical Co., Ltd.'s offer)；Paeoniflorin is compareed
Product (Chengdu Man Site bio tech ltd, lot number：MUST-11030608)；Acetonitrile (Merck, Germany)；Phosphoric acid
(Aladdin)；Heartily pure water.
1.2 key instruments and equipment
Agilent1200 high performance liquid chromatographs (Agilent1200 pumps, Agilent1200 photo-diode array detections
Device, Agilent1200 chromatographic work stations, Agilent Technologies of the U.S.)；Antaris ft-nir spectrometers
(Thermo Nicolet, USA)；Equipped with corresponding transmission detector annex sampling system and signal acquisition and Result,
The data processing softwares such as TQAnalyst；Sartorius CP225D electronic analytical balances (the limited public affairs of Beijing Sai Duolisi balances
Department)；RE-52AA Rotary Evaporators (Shanghai Yarong Biochemical Instrument Plant)；(Zhejiang temperature brother's mechanical valve industry has 40L multi-function extractors
Limit company)；HS6150 types ultrasonic cleaner (Tianjin perseverance AudioCodes skill Development Co., Ltd).
2. method and result
The collection of 2.1 aqueous extract samples
4kg medicinal materials comprising the root of herbaceous peony, radix bupleuri, corydalis tuber and radix glycyrrhizae are put into volume in 40L multi-function extractor, to press
A pan-fried, two pan-fried extractions are carried out according to production technology.In order to which the sample concentration for ensureing gathered is uniformly distributed, during one decocts, immersion
Stage is sampled once per 10min, is sampled once per 8min in the heating period, and preceding 30min is sampled once per 6min in boiling process
Remaining time samples once per 10min；Two decoct during the heating period per 8min sample once, boiling process per 10min sample
Once, 7 batch water extraction experiments are carried out altogether.210 samples are obtained after the completion of all batch experiments.By the 1st, 2,3,5,6,7
The extract solution sample of secondary experiment is as calibration set, and the 4th is extracted sample and collected as checking.
2.2 near infrared spectra collection
The transmitted spectrum of the extract solution sample of the water extraction process of qizhi weitong granules is gathered, the scanning range of spectrum is set
4000~10000cm-1, scanning times are 32 times, and resolution ratio is 8cm-1, using air as background, using the cylinder of 5mm light paths
Glass colorimetric cylinder, the water of (temperature is 25 DEG C, and humidity is 35%-45%) collection qizhi weitong granules in a constant environment
The extract solution transmitted spectrum of extraction process, each sample replication 3 times calculates averaged spectrum.The water extraction of qizhi weitong granules
Take the original atlas of near infrared spectra of process as shown in Figure 1.
By the automatic majorization function of OPUS softwares, 5448.8~6102.7cm is filtered out-1And 7498.9-8451.5cm-1
Two wave bands, while choosing 6201~6501cm according to spectrum change trend-1Between wave band carry out model foundation, pass through optimization
Compare, finally select 5448.8~6102.7cm-1And 6201-6501cm-1Two wave bands are set up water extraction process Paeoniflorin and quantified
Detection model.The modeling wave band provided according to TQ softwares, 6201~5701cm is selected for solid content model-1With 7170~
7300cm-1Two wave bands carry out quantitative model foundation.And using single order, second dervative processing, smooth, vector normalizing, scattering effect
Should correct, multiple linear correction, a variety of chemometrics methods such as wavelet transformation, this model is set up is led using single order, second order
The method that number processing combines S-G or Norris smothing filterings is pre-processed to spectrum.
Tables 1 and 2 is respectively using setting up the near red of Paeoniflorin and solid content after original spectrum and different pretreatments method
The R that outer quantitative calibration models are obtained2, RMSEC, RMSECV value, by comparing the model that different pretreatments method is set up
RMSEC and RMSECV values determine preprocess method.
The water extraction process Paeoniflorin of the different pretreatments method of table 1 quantitative determines the parameter of model
The water extraction process solid content of the different pretreatments method of table 2 quantitative determines the parameter of model
As shown in Table 1, water extraction process Paeoniflorin quantitative determination model preprocess method using first derivative processing+
During the method for Norris smothing filterings, RMSECV values and RMSEC values are minimum；As shown in Table 2, water extraction process solid content is quantitatively surveyed
When the preprocess method of cover half type uses the method for first derivative processing+Norris smothing filterings, RMSECV values and RMSEC values are most
It is small.Quantitative model is calculated using PLS (PLSR).
2.3 paeoniflorin contents are determined
By the above-mentioned extract solution sample centrifugation 10min (13000r/min) collected, supernatant is pipetted, HPLC contents are carried out
Determine.HPLC chromatogram condition is as follows：Chromatographic column：Agilent Zorbax SB-C18 (4.6 × 250mm, 5 μm)；Mobile phase：
0.1% phosphoric acid water (A)-acetonitrile (B)；Sample size：5μL；Flow velocity：1.0mL/min；Column temperature：30℃；Detection wavelength：230nm.Wash
De- Gradient program is as shown in table 3.
The gradient elution program of table 3
Analyzed by 2.3 chromatographic conditions, sample size is 5 μ L, determines the content of different batches Paeoniflorin, the results are shown in Table shown in 4.
The HPLC chromatogram of Paeoniflorin reference substance is as shown in Fig. 2 the HPLC chromatogram of Paeoniflorin sample is as shown in Figure 3.
The water extraction process paeoniflorin content measurement result of table 4
2.4 determination of solid content
Extract solution stand 24h, measure 4mL supernatants to dried to constant weight flat bottle (twice dry after weight difference away from
Less than 5mg) (X0), weigh (X1), put and dry under the conditions of 105 DEG C of baking oven to weight difference of weighing twice away from less than 5mg, count X2。
Solid content (%)=(X2-X0)/(X1-X0) × 100%
By 2.4 determination of solid content methods, the solid content of different batches aqueous extract is determined, as a result as shown in table 5.
The water extraction process determination of solid content result of table 5
The foundation of 2.5 quantitative models
The wave band and Pretreated spectra side for selecting optimum modeling set up water extraction process Paeoniflorin, solid content and quantitatively detect mould
Type.The near-infrared predicted value of Paeoniflorin calibration set sample is with the dependency relation figure of efficient liquid phase measured value as shown in figure 4, solid content
The near-infrared predicted value of calibration set sample and the dependency relation figure of measured value are as shown in Figure 5.Near-infrared is predicted as can be seen from Figure
Value is good with correlation between measured value, and measurement result reaches unanimity substantially, and the parameter of gained model is as shown in table 6.Can by table 6
Know, Paeoniflorin and solid content model calibration set coefficient R2Respectively up to 0.97686,0.99633, RMSEC be respectively 0.0645,
0.0541, now corresponding RMSECV is minimum.
The quantitative detection model parameter of the water extraction process of table 6
2.6 water extract course prediction
The sample of the 4th batch of extraction is predicted with the calibration model set up, the near-infrared of Paeoniflorin checking collection sample
The dependency relation figure of predicted value and HPLC measured values is as shown in fig. 6, the near-infrared predicted value of solid content checking collection sample is with determining
The dependency relation figure of value is as shown in Figure 7.Paeoniflorin, solid content forecast set coefficient R2Respectively 0.96859,0.99743, can
See between predicted value and control value there is good correlation, model has preferable performance.Paeoniflorin, solid content RMSEP are respectively
0.0623rd, 0.0533, Paeoniflorin, the RSEP of solid content are respectively 6.83%, 3.78%, control within 10%, disclosure satisfy that
The required precision of the real-time monitoring analysis of Chinese Traditional Medicine.
Water extraction process one decoct the change in concentration compares figure of liquid chromatogram measuring and model prediction Paeoniflorin as shown in figure 8,
Water extraction process one decocts determination of solid content and changes compares figure as shown in figure 9, the decocting liquid of water extraction process two with model prediction solid content
The change in concentration compares figure of phase chromatographic determination and model prediction Paeoniflorin is as shown in Figure 10, and water extraction process two decocts determination of solid content
It is as shown in figure 11 with model prediction solid content change compares figure.
From Fig. 8~Figure 11, the near-infrared predicted value that model is obtained is kept substantially with Paeoniflorin, determination of solid content value
Unanimously, the process trend of its predicted value is also substantially the same with real process；The constituent concentration height of sample is near infrared spectrum skill
The influence of art estimated performance is larger, and the high prediction effect of concentration is significantly better than low concentration.
After Paeoniflorin, solid content calibration model are established, using institute's construction method, NIRS, which completes one-shot measurement, only to be needed 20 seconds, and
Efficient liquid phase completes 1 paeoniflorin content and determined at least to need 30min, determination of solid content then at least some hours.Therefore use
Near-infrared spectral analysis technology can not only realize the real-time monitoring of extraction of traditional Chinese medicine active constituent content and solid content, and
The detection method is easier than conventional method, more rapidly.
Embodiment 2Near-infrared spectrum technique is used in qizhi weitong granules preparation process the research for extracting volatile oil process
1. instrument and reagent
1.1 main Chinese medicinal materials and reagent
Fructus Aurantii, rhizoma cyperi (processing), Liaoning Huarun Benxi Third Pharmaceutical Co., Ltd. provide；Neohesperidin reference substance (Chengdu Man Site
Bio tech ltd, lot number：MUST-11030701)；Aurantiin reference substance (Chengdu Man Site bio tech ltd,
Lot number：MUST-11030612)；Acetonitrile (Merck, Germany)；Phosphoric acid (Aladdin)；Heartily pure water.
1.2 key instruments and equipment
1.2 contents under be the same as Example 1.
2. method and result
The collection of 2.1 extract solution samples
12kg medicinal materials comprising Fructus Aurantii, rhizoma cyperi are put into volume in 40L multi-function extractor, according to production technology to enter
Row is extracted.In order to which the sample concentration for ensureing gathered is uniformly distributed, impregnation stage is sampled once per 10min, every in the heating period
8min is sampled once, and preceding 60min samples once remaining time every 10min per 6min and sampled once in boiling process.6 are carried out altogether
Batch extracts volatile oil experiment.198 samples are obtained after the completion of all batch experiments.By the 1st, 2,3,5,6 experiments carry
Take liquid sample as calibration set, the 4th is extracted sample and collected as checking.
The collection of 2.2 near infrared spectrums
Gather the transmitted spectrum that qizhi weitong granules extracts volatile oil procedure extraction liquid sample：Set the scanning range of spectrum
4000~10000cm-1, scanning times are 32 times, and resolution ratio is 8cm-1, using air as background, using the cylinder of 5mm light paths
Glass colorimetric cylinder, (temperature is 25 DEG C, and humidity is 35%-45%) collection qizhi weitong granules is extracted in a constant environment
The extract solution transmitted spectrum of volatile oil process, each sample replication 3 times calculates averaged spectrum.Qizhi weitong granules is extracted
During extract oil part original near infrared spectrum it is as shown in figure 12.
The quality of model is set up by the wave band for comparing TQ optimum choices wave band and being selected according to correlation coefficient process, most
5500~6100cm is selected eventually-1With 7170~7270cm-1, 5500~6100cm-1And 5600~6000cm-1Respectively as shaddock
The quantitative detection model modeling wave band of skin glycosides, neohesperidin and solid content；And using single order, second dervative processing, smooth, arrow
A variety of chemometrics methods such as normalizing, scattering effect correction, multiple linear correction, wavelet transformation are measured, this model is set up and adopted
The method for combining S-G or Norris smothing filterings with single order, second dervative processing is pre-processed to spectrum.Table 7, the and of table 8
Table 9 is respectively to be determined using the near-infrared that aurantiin, neohesperidin and solid content are set up after original spectrum and different pretreatments method
The R that amount calibration model is obtained2, RMSEC, RMSECV value, by compare the model that different pretreatments method is set up RMSEC and
RMSECV values determine preprocess method.
The parameter of the quantitative detection model of aurantiin of the extraction volatile oil process of the different pretreatments method of table 7
The parameter of the quantitative detection model of neohesperidin of the extraction volatile oil process of the different pretreatments method of table 8
The parameter of the quantitative detection model of solid content of the extraction volatile oil process of the different pretreatments method of table 9
From table 7, table 8 and table 9, set up comparing different pretreatments method in PLS calibration models, aurantiin with
And the light after the method processing of the RMSECV values and RMSEC values of neohesperidin to handle+Norris smothing filterings through first derivative
It is minimum during spectrum modeling, at the method for the RMSECV values and RMSEC values of solid content to handle+S-G smothing filterings through first derivative
It is minimum when spectrum after reason is modeled.Accordingly, it is determined that handling the method for+Norris smothing filterings to aurantiin using first derivative
And neohesperidin model spectrum is pre-processed；The method of+S-G smothing filterings is handled to solid content model using first derivative
Spectrum is pre-processed；Quantitative model is calculated using PLS (PLSR).
The assay of 2.3 aurantiamarins, aurantiin
By the above-mentioned extract solution sample centrifugation 10min (13000r/min) collected, supernatant is pipetted, HPLC contents are carried out
Determine, HPLC chromatogram condition is as follows：
Chromatographic column：Agilent Zorbax SB-C18 (4.6 × 250mm, 5 μm)；
Mobile phase：0.1% phosphoric acid water (A)-acetonitrile (B)；Sample size：5μL；
Flow velocity：1.0mL/min；Column temperature：30℃；Detection wavelength：283nm；
As shown in table 10, assay result is as shown in table 11 for gradient program.
The gradient elution program of table 10
Table 11 extracts the aurantiin of volatile oil process, neohesperidin assay result
2.4 determination of solid content
Extract solution stand 24h, measure 4mL supernatants to dried to constant weight flat bottle (twice dry after weight difference away from
Less than 5mg) (X0), weigh (X1), put and dry under the conditions of 105 DEG C of baking oven to weight difference of weighing twice away from less than 5mg, count X2。
Solid content (%)=(X2-X0)/(X1-X0) × 100%
By 2.4 determination of solid content methods, the solid content that different batches extract the sample liquid of volatile oil process, solid content are determined
Measurement result is as shown in table 12.
Table 12 extracts the determination of solid content result of volatile oil process
The foundation of 2.5 quantitative models
Aurantiin, new orange peel during the wave band and preprocessing procedures foundation extraction volatile oil of selection optimum modeling
The quantitative detection model of glycosides, solid content, the parameter of gained model is as shown in table 13.The near-infrared predicted value of aurantiin calibration set sample
Dependency relation figure with efficient liquid phase measured value is as shown in figure 13, the near-infrared predicted value of neohesperidin aurantiin calibration set sample
Dependency relation figure with efficient liquid phase measured value is as shown in figure 14, the near-infrared predicted value and measured value of solid content calibration set sample
Dependency relation figure it is as shown in figure 15.
From Figure 13~Figure 15, correlation is good between the near-infrared predicted value and measured value of aurantiin and neohesperidin
Good, measurement result reaches unanimity substantially；Correlation is good between the near-infrared predicted value and measured value of solid content, measurement result base
Originally reach unanimity.As shown in Table 13, aurantiin, neohesperidin and solid content model calibration set coefficient R2Reach respectively
0.99302nd, 0.99267,0.99716, RMSEC is respectively 0.269,0.124,0.159, RMSECV is corresponded to herein minimum.
Table 13 extracts the quantitative detection model parameter of volatile oil process
2.6 extract volatile oil course prediction
The sample of the 4th batch of extraction is predicted with the calibration model set up, the near-infrared of aurantiin checking collection sample
The dependency relation figure of predicted value and efficient liquid phase measured value is as shown in figure 16, the near-infrared predicted value of neohesperidin checking collection sample
Dependency relation figure with HPLC measured values is as shown in figure 17, the phase of the near-infrared predicted value and measured value of solid content checking collection sample
Close graph of a relation as shown in figure 18.From Figure 16~Figure 18, aurantiin, neohesperidin, solid content forecast set coefficient R2Point
Wei 0.99345,0.99843,0.99816, it is seen that have good correlation between predicted value and control value, model has preferably
Performance；Aurantiin, neohesperidin, solid content RMSEP are respectively 0.265,0.162,0.305, aurantiin, neohesperidin, are contained admittedly
The RSEP of amount is respectively 5.71%, 7.73%, 6.66%, controls within 10%, disclosure satisfy that Chinese Traditional Medicine is supervised in real time
Control the required precision of analysis.
Extract the liquid chromatogram measuring of volatile oil process and change in concentration compares figure such as Figure 19 institutes of model prediction aurantiin
Show, the change in concentration compares figure for extracting the liquid chromatogram measuring and model prediction neohesperidin of volatile oil process is as shown in figure 20,
The determination of solid content and model prediction solid content change compares figure for extracting volatile oil process are as shown in figure 21.Can by Figure 19~Figure 21
Know, the near-infrared predicted value that model is obtained is consistent substantially with aurantiin, neohesperidin, determination of solid content value, it is predicted
The process trend of value is also substantially the same with real process；In addition, the constituent concentration height of sample is predicted near-infrared spectrum technique
Performance impact is larger, and the high prediction effect of concentration is significantly better than low concentration.
After aurantiin, neohesperidin, the calibration model of solid content are established, using institute's construction method, NIRS completes one-shot measurement
Only need 20 seconds, and efficient liquid phase completes 1 aurantiin, neohesperidin assay at least needs 30min, determination of solid content is then extremely
Few some hours.Therefore, can not only be realized using near-infrared spectral analysis technology extraction of traditional Chinese medicine active constituent content and
The real-time monitoring of solid content, and its detection method is easier than conventional method, more rapidly.
Embodiment 3Near-infrared spectrum technique is used for the research of extract solution concentration process in qizhi weitong granules preparation process
1st, experiment material
1.1 medicinal materials and reagent
Qizhi weitong granules concentrate (Liaoning Huarun Benxi Third Pharmaceutical Co., Ltd.'s offer)；(Chengdu is graceful for Paeoniflorin reference substance
Si Te bio tech ltd, lot number：MUST-11030608)；Acetonitrile (Merck, Germany)；Phosphoric acid (Aladdin)；
Heartily pure water.
1.2 key instruments and equipment
1.2 contents under be the same as Example 1.
2. method and result
The collection of 2.1 concentrate samples
Because the medicine workshop concentrator (coiled vacuum concentration pan) of Liaoning China Resources Benxi three can in concentration process
To take out concentrate sample, concentration process sample is in Liaoning Huarun Benxi Third Pharmaceutical Co., Ltd.'s workshop collection in worksite.Extract
The standing filtered fluid of liquid input disc tube type vacuum concentration pan and when reaching default thickening temperature and pressure as time zero
And starting sampling, sample volume is 50mL.Often sample every other hour within first 8 hours or so.Concentration in all single-action and economic benefits and social benefits
Liquid is input to after coiled vacuum concentration pan every sampling in 20 minutes once, until going out cream, repeats 10 batches.All batches are real
120 samples are obtained after the completion of testing.Using the 1st, the concentrate samples of 2,3,4,6,7,8,9,10 experiments as calibration set, the
5 concentrate samples collect as checking.
2.2 near infrared spectra collection
Gather the transmitted spectrum of qizhi weitong granules concentrate：Set 4000~10000cm of scanning range of spectrum-1, sweep
Number of times is retouched for 32 times, resolution ratio is 8cm-1, using air as background, using the cylindrical glass colorimetric cylinder of 5mm light paths, in a perseverance
In fixed environment (temperature be 25 DEG C, humidity be 35%~45%) gather qizhi weitong granules concentrate transmitted spectrum, each sample
Product replication 3 times, calculates averaged spectrum.The original near infrared spectrum of qizhi weitong granules concentrate is as shown in figure 22.
A series of wave bands have selected using TQ, OPUS and correlation coefficient process respectively, by comparing each wave band and not
With the modeling effect of band combination, 5449.8~6101.7cm is finally selected-1, 5149.01~5442.13cm-1With 5469.13
~7143.04cm-1, 5149.01~5442.13cm-1With 5469.13~7143.04cm-1Respectively as Paeoniflorin, it is relatively close
Degree, the modeling wave band of solid content, and using single order, second dervative processing, smooth, vector normalizing, scattering effect correction, polynary line
Property a variety of chemometrics methods such as correction, wavelet transformation, this model is set up combines S-G using single order, second dervative processing
Or the method for Norris smothing filterings is pre-processed to spectrum, using setting up Chinese herbaceous peony after original spectrum and different pretreatments method
The R that medicine glycosides, relative density, the near-infrared quantitative calibration models of solid content are obtained2, RMSEC, RMSECV value is respectively such as table 14, table
15 and table 16 shown in, by compare the model that different pretreatments method is set up RMSEC and RMSECV values determine pretreatment side
Method.
The parameter of the quantitative detection model of the extract solution concentration process Paeoniflorin of the different pretreatments method of table 14
The quantitative detection model parameter of the relative density of the extract solution concentration process of the different pretreatments method of table 15
The quantitative detection model parameter of the solid content of the extract solution concentration process of the different pretreatments method of table 16
From table 14, table 15 and table 16, different pretreatments method is set up in PLS calibration models, Paeoniflorin
RMSECV values and RMSEC values through second dervative to handle during the spectrum modeling after the method for+Norris smothing filterings is handled as most
It is small, at the method for the RMSECV values and RMSEC values of relative density and solid content to handle+Norris smothing filterings through first derivative
It is minimum when spectrum after reason is modeled.Therefore, the method for+Norris smothing filterings is handled using second dervative to Paeoniflorin model
Spectrum is pre-processed, and the method for+Norris smothing filterings is handled to relative density and solid content model light using first derivative
Spectrum is pre-processed；Quantitative model is calculated using PLS (PLSR).
2.3 paeoniflorin contents are determined
By the above-mentioned extract solution sample centrifugation 10min (13000r/min) collected, supernatant is pipetted, according to sample concentration
With 5 times or 10 times of distilled water diluting, HPLC assays are carried out, HPLC conditions are as follows：
Chromatographic column：Agilent Zorbax SB-C18 (4.6 × 250mm, 5 μm)；
Mobile phase：0.1% phosphoric acid water (A)-acetonitrile (B)；Sample size：5μL
Flow velocity：1.0mL/min；Column temperature：30℃；Detection wavelength：230nm；
Gradient program is shown in Table 17.
The gradient elution program of table 17
Analyzed by 2.3 chromatographic conditions, sample size is 5 μ L, determines the content of different batches Paeoniflorin.Containing for Paeoniflorin is measured
Determine result as shown in table 18, the HPLC collection of illustrative plates of Paeoniflorin reference substance is as shown in figure 23, HPLC collection of illustrative plates such as Figure 24 of Paeoniflorin sample
It is shown.
The paeoniflorin content measurement result of the extract solution concentration process of table 18
2.4 relative density determination
Supernatant is pipetted after concentrate sample centrifugation (13000r/min, 10min), constant temperature in 50 DEG C of water-baths is placed in and keeps
30min.Precision pipettes 1mL supernatant samples, weighs, and institute's value is concentrating sample relative density values (g/mL), by 2.4 phases
To density measurement method, the relative density of different batches concentrate is determined, 19 are the results are shown in Table.
The relative density determination result of the extract solution concentration process of table 19
2.5 determination of solid content
Extract solution stand 24h, measure 4mL supernatants to dried to constant weight flat bottle (twice dry after weight difference away from
Less than 5mg) (X0), weigh (X1), put and dry under the conditions of 105 DEG C of baking oven to weight difference of weighing twice away from less than 5mg, count X2。
Solid content (%)=(X2-X0)/(X1-X0) × 100%
By " 2.5 determination of solid content " method, the solid content of different batches concentrate, the assay result such as institute of table 20 are determined
Show.
The determination of solid content result of the extract solution concentration process of table 20
The foundation of 2.6 quantitative models
The wave band and Pretreated spectra side for selecting optimum modeling set up the Paeoniflorin of extract solution concentration process, relative density,
The quantitative detection model of solid content, the parameter of gained model is as shown in table 21.The near-infrared predicted value of Paeoniflorin calibration set sample with
The dependency relation figure of efficient liquid phase measured value is as shown in figure 25, the near-infrared predicted value and measured value of relative density calibration set sample
Dependency relation figure as shown in figure 26, the near-infrared predicted value of solid content calibration set sample and the dependency relation figure of measured value are as schemed
Shown in 27.Correlation is good between Figure 25~Figure 27, near-infrared predicted value and measured value, and measurement result tends to one substantially
Cause.As shown in Table 21, Paeoniflorin, relative density, solid content model calibration set coefficient R2Respectively up to 0.98125,
0.99551st, 0.99977, RMSEC is respectively 0.597,0.00584,0.247, now corresponds to RMSECV minimum.
The quantitative detection model parameter of the extract solution concentration process of table 21
2.7 extract solution concentration process are predicted
The sample of the 5th batch of extraction is predicted with the calibration model set up, the near-infrared of Paeoniflorin checking collection sample
The dependency relation figure of predicted value and HPLC measured values is as shown in figure 28, and the near-infrared predicted value of relative density checking collection sample is with surveying
As shown in figure 29, solid content checking collects the near-infrared predicted value of sample and the dependency relation figure of measured value to the dependency relation figure of definite value
As shown in figure 30.From Figure 28~Figure 30, Paeoniflorin, relative density, solid content forecast set coefficient R2Respectively
0.99859th, 0.99876,0.99743, this shows, there is good correlation between predicted value and control value, and model has preferably
Performance；Paeoniflorin, relative density, the RMSEP of solid content are respectively 0.407,0.00677,0.436, Paeoniflorin, relative density,
The RSEP of solid content is respectively 7.10%, 0.62%, 1.86%, is controlled within 10%, disclosure satisfy that Chinese Traditional Medicine is real
When monitoring analysis required precision.
The change in concentration compares figure of extract solution concentration process determination of solid content and model prediction solid content is as shown in figure 31, carries
Take the change in concentration compares figure of liquid concentration process relative density determination and model prediction relative density as shown in figure 32, extract solution is dense
The change in concentration compares figure of compression process determination of solid content and model prediction solid content is as shown in figure 33.From Figure 31~Figure 33,
The near-infrared predicted value that model is obtained is consistent substantially with Paeoniflorin, relative density, determination of solid content value, its predicted value
Process trend is also substantially the same with real process.
After Paeoniflorin, relative density, solid content calibration model are established, using institute's construction method, NIRS completes one-shot measurement only
Need 20 seconds, and efficient liquid phase completes 1 paeoniflorin content and determined at least to need 30min, relative density, determination of solid content are then at least
Some hours.Therefore, extraction of traditional Chinese medicine active constituent content and solid content can be not only realized using near infrared spectroscopy
Monitoring in real time, and its detection method is easier than conventional method, more rapidly.
To sum up, the present invention establish qizhi weitong granules preparation process reclaimed water extraction process, extract volatile oil process and
The on-line near infrared spectroscopy analysis method of extract solution concentration process, and it is applied to on-line checking, realize energy-stagnation stomachache
The automatic detection of the preparation process of grain and the real-time estimate of each quality control index content；The model prediction accuracy set up is high, accurate
Exactness is high, meets the requirement of quantitative analysis in actual production.
Obviously, above-described embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (9)
1. a kind of method of the preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules, it is characterised in that
The extraction volatile oil process of the detection of water extraction process including following qizhi weitong granules and/or qizhi weitong granules
The detection of the extract solution concentration process of detection and/or qizhi weitong granules：
A, the water extraction process of qizhi weitong granules detection
The step of assay and/or determination of solid content including following Paeoniflorin:
A, the assay of Paeoniflorin comprise the following steps：
(1) aqueous extract of the qizhi weitong granules of known paeoniflorin content is taken, it is standby；
(2) aqueous extract of the qizhi weitong granules is subjected near infrared spectrum scanning, gathers the qizhi weitong granules
The near infrared spectrum of aqueous extract；
(3) 5448.8~6102.7cm is chosen-1With 6201~6501cm-1Spectral information under characteristic wave bands, applied chemistry metering
The paeoniflorin content for learning software and the aqueous extract of the qizhi weitong granules of the known paeoniflorin content is associated, using inclined
The quantitative calibration model that least square method is set up between near infrared spectrum and standard content；
(4) near infrared spectrum is carried out to the aqueous extract sample of unknown qizhi weitong granules according to the method for the step (2) to sweep
Retouch, and choose 5448.8~6102.7cm-1With 6201~6501cm-1Spectral information under characteristic wave bands, imports quantifying for foundation
Calibrating patterns obtain the paeoniflorin content value of the aqueous extract sample of the unknown qizhi weitong granules；
B, determination of solid content comprise the following steps：
(1) aqueous extract of the qizhi weitong granules of known solid content is taken, it is standby；
(2) aqueous extract of the qizhi weitong granules is subjected near infrared spectrum scanning, gathers the qizhi weitong granules
The near infrared spectrum of aqueous extract；
(3) 6201~5701cm is chosen-1With 7170~7300cm-1Spectral information under characteristic wave bands, Applied Chemometrics is soft
The solid content of part and the aqueous extract of the qizhi weitong granules of the known solid content is associated, and is built using PLS
Vertical quantitative calibration model between near infrared spectrum and standard content；
(4) near infrared spectrum is carried out to the aqueous extract sample of unknown qizhi weitong granules according to the method for the step (2) to sweep
Retouch, and choose 6201~5701cm-1With 7170~7300cm-1Spectral information under characteristic wave bands, imports the quantitative calibration set up
Model obtains the solid content value of the aqueous extract sample of the unknown qizhi weitong granules；
B, the extraction volatile oil process of qizhi weitong granules detection
The step of assay and/or determination of solid content of assay, neohesperidin including following aurantiin:
A, the assay of aurantiin comprise the following steps：
(1) extract solution of the extraction volatile oil process of the qizhi weitong granules of known naringin content is taken, it is standby；
(2) extract solution of the extraction volatile oil process of the qizhi weitong granules is subjected near infrared spectrum scanning, collection is described
The near infrared spectrum of the extract solution of the extraction volatile oil process of qizhi weitong granules；
(3) 5500~6100cm is chosen-1Spectral information under characteristic wave bands, Applied Chemometrics software and the known shaddock ped
The naringin content of the extract solution of the extraction volatile oil process of the qizhi weitong granules of glycosides content is associated, using a most young waiter in a wineshop or an inn partially
The quantitative calibration model that multiplication is set up between near infrared spectrum and standard content；
(4) the extract solution sample of the extraction volatile oil process of unknown qizhi weitong granules is entered according to the method for the step (2)
Row near infrared spectrum scanning, and choose 5500~6100cm-1Spectral information under characteristic wave bands, imports the quantitative calibration mould set up
Type obtains the naringin content value of the extract solution sample of the extraction volatile oil process of the unknown qizhi weitong granules；
B, the assay of neohesperidin comprise the following steps：
(1) extract solution of the extraction volatile oil process of the qizhi weitong granules of known neohesperidin content is taken, it is standby；
(2) extract solution of the extraction volatile oil process of the qizhi weitong granules is subjected near infrared spectrum scanning, collection is described
The near infrared spectrum of the extract solution of the extraction volatile oil process of qizhi weitong granules；
(3) 7170~7270cm is chosen-1With 5500~6100cm-1Spectral information under characteristic wave bands, Applied Chemometrics is soft
The neohesperidin content of part and the extract solution of the extraction volatile oil process of the qizhi weitong granules of the known neohesperidin content
It is associated, the quantitative calibration model set up using PLS between near infrared spectrum and standard content；
(4) the extract solution sample of the extraction volatile oil process of unknown qizhi weitong granules is entered according to the method for the step (2)
Row near infrared spectrum scanning, and choose 7170~7270cm-1With 5500~6100cm-1Spectral information under characteristic wave bands, is imported
The quantitative calibration model of foundation obtains the new orange of the extract solution sample of the extraction volatile oil process of the unknown qizhi weitong granules
Skin glycosides content value；
C, determination of solid content comprise the following steps：
(1) extract solution of the extraction volatile oil process of the qizhi weitong granules of known solid content is taken, it is standby；
(2) extract solution of the extraction volatile oil process of the qizhi weitong granules is subjected near infrared spectrum scanning, collection is described
The near infrared spectrum of the extract solution of the extraction volatile oil process of qizhi weitong granules；
(3) 5600~6000cm is chosen-1Spectral information under characteristic wave bands, Applied Chemometrics software known contains admittedly with described
The solid content of the extract solution of the extraction volatile oil process of the qizhi weitong granules of amount is associated, and is set up using PLS
Quantitative calibration model between near infrared spectrum and standard content；
(4) the extract solution sample of the extraction volatile oil process of unknown qizhi weitong granules is entered according to the method for the step (2)
Row near infrared spectrum scanning, and choose 5600~6000cm-1Spectral information under characteristic wave bands, imports the quantitative calibration mould set up
Type obtains the solid content value of the extract solution sample of the extraction volatile oil process of the unknown qizhi weitong granules；
C, the extract solution concentration process of qizhi weitong granules detection
The step of assay, relative density and/or determination of solid content including following Paeoniflorin:
A, the assay of Paeoniflorin comprise the following steps：
(1) concentrated extracting solution of the qizhi weitong granules of known paeoniflorin content is taken, it is standby；
(2) concentrated extracting solution of the qizhi weitong granules is subjected near infrared spectrum scanning, gathers the qizhi weitong granules
Concentrated extracting solution near infrared spectrum；
(3) 5449.8~6101.7cm is chosen-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands, application
The paeoniflorin content for learning meterological software and the concentrated extracting solution of the qizhi weitong granules of the known paeoniflorin content is closed
Connection, the quantitative calibration model set up using PLS between near infrared spectrum and standard content；
(4) near infrared spectrum is carried out to the concentrated extracting solution sample of unknown qizhi weitong granules according to the method for the step (2)
Scanning, and choose 5449.8~6101.7cm-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands, importing is built
Vertical quantitative calibration model obtains the paeoniflorin content value of the concentrated extracting solution sample of the unknown qizhi weitong granules；
B, relative density determination comprise the following steps：
(1) concentrated extracting solution of the qizhi weitong granules of known relative density is taken, it is standby；
(2) concentrated extracting solution of the qizhi weitong granules is subjected near infrared spectrum scanning, gathers the qizhi weitong granules
Concentrated extracting solution near infrared spectrum；
(3) 5469.13~7143.04cm is chosen-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands, application
The relative density of chemo metric software and the concentrated extracting solution of the qizhi weitong granules of the known relative density is associated,
The quantitative calibration model set up using PLS between near infrared spectrum and standard content；
(4) near infrared spectrum is carried out to the concentrated extracting solution sample of unknown qizhi weitong granules according to the method for the step (2)
Scanning, and choose 5469.13~7143.04cm-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands, is imported
The quantitative calibration model of foundation obtains the relative density values of the concentrated extracting solution sample of the unknown qizhi weitong granules；
C, determination of solid content comprise the following steps：
(1) concentrated extracting solution of the qizhi weitong granules of known solid content is taken, it is standby；
(2) concentrated extracting solution of the qizhi weitong granules is subjected near infrared spectrum scanning, gathers the qizhi weitong granules
Concentrated extracting solution near infrared spectrum；
(3) 5469.13~7143.04cm is chosen-1Spectral information under characteristic wave bands, Applied Chemometrics software with it is described
Know that the solid content of the concentrated extracting solution of the qizhi weitong granules of solid content is associated, near-infrared is set up using PLS
Quantitative calibration model between spectrum and standard content；
(4) near infrared spectrum is carried out to the concentrated extracting solution sample of unknown qizhi weitong granules according to the method for the step (2)
Scanning, and choose 5469.13~7143.04cm-1Spectral information under characteristic wave bands, imports the quantitative calibration model set up and obtains
The solid content value of the concentrated extracting solution sample of the unknown qizhi weitong granules.
2. the side of the preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules according to claim 1
Method, it is characterised in that
It is in the step of assay of Paeoniflorin in the detection of the water extraction process of the qizhi weitong granules (2) and/or solid
In the step of assay (2), the near-infrared of the aqueous extract of the qizhi weitong granules is carried out using static spectrum acquisition method
Spectra collection, actual conditions is：Spectral acquisition times are at intervals of 10min, using air as reference, and scanning times are 32 times, are differentiated
Rate is 8cm-1, scanning optical spectrum scope is 4000~10000cm-1；
In the step of assay of aurantiin in the detection of the extraction volatile oil process of the qizhi weitong granules (2), newly
In the step of assay of aurantiamarin (2) and/or the step of determination of solid content in (2), carried out using static spectrum acquisition method
The near infrared spectra collection of the extraction volatile oil process of the qizhi weitong granules, actual conditions is：Spectral acquisition times interval
For 10min, using air as reference, scanning times are 32 times, and resolution ratio is 8cm-1, scanning optical spectrum scope is 4000~10000cm-1；
The step of assay of Paeoniflorin in the detection of the extract solution concentration process of the qizhi weitong granules (2) neutralization/
Or in the step of determination of solid content (2), the concentrated extracting solution of the qizhi weitong granules is carried out using static spectrum acquisition method
Near infrared spectra collection, actual conditions is：Spectral acquisition times are at intervals of 10min, using air as reference, and scanning times are 32
Secondary, resolution ratio is 8cm-1, scanning optical spectrum scope is 4000~10000cm-1。
3. the preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules according to claim 1 or 2
Method, it is characterised in that
It is in the step of assay of Paeoniflorin in the detection of the water extraction process of the qizhi weitong granules (2) and/or solid
In the step of assay (2), in addition to First derivative spectrograply and Norris derivatives are used to the near infrared spectrum collected
The step of smothing filtering method is pre-processed；
(2) neutralization of the step of assay of aurantiin in the detection of the extraction volatile oil process of the qizhi weitong granules/
Or neohesperidin assay the step of (2) in, in addition to First derivative spectrograply is used to the near infrared spectrum collected
The step of being pre-processed with Norris derivative smoothing filter methods；
The qizhi weitong granules extraction volatile oil process detection in determination of solid content the step of (2) in, in addition to pair
The step of near infrared spectrum collected is pre-processed using First derivative spectrograply and S-G smothing filtering methods；
In the step of assay of Paeoniflorin in the detection of the extract solution concentration process of the qizhi weitong granules (2), also
Pre-processed including the near infrared spectrum to collecting using second derivative method and Norris derivative smoothing filter methods
Step；
In the step of relative density in the detection of the extract solution concentration process of the qizhi weitong granules (2) and/or solid content
In the step of measure (2), in addition to First derivative spectrograply and Norris derivative smoothings are used to the near infrared spectrum collected
The step of filter method is pre-processed.
4. the preparation of the utilization near infrared spectroscopy quick detection qizhi weitong granules according to claim any one of 1-3
The method of journey, it is characterised in that
The bulk drug of the qizhi weitong granules is constituted：
The parts by weight of radix bupleuri 30~100, the parts by weight of radix glycyrrhizae 15~60, the parts by weight of rhizoma cyperi 35~120, the parts by weight of corydalis tuber 35~120,
The parts by weight of the root of herbaceous peony 40~150, the parts by weight of Fructus Aurantii 35~120.
5. the preparation of the utilization near infrared spectroscopy quick detection qizhi weitong granules according to claim any one of 1-4
The method of journey, it is characterised in that
The preparation method of the qizhi weitong granules comprises the following steps：
(1) Fructus Aurantii and rhizoma cyperi of selected parts by weight are taken, volatile oil is extracted, decoction is standby, and the dregs of a decoction are discarded；
(2) radix bupleuri, radix glycyrrhizae, corydalis tuber and the root of herbaceous peony of selected parts by weight are taken, is added water to cook 2 times, the 1st decoction 0.5~4 hour,
2nd decoction 0.5~3 hour；
(3) combining step (1) and the decocting liquid of step (2), filtering, filtrate are concentrated into the clear cream that relative density is 1.10~1.30；
(4) particle is made in qinghuo reagent, plus auxiliary material, mixing, dries, and sprays into volatile oil, produces granule.
6. the preparation of the utilization near infrared spectroscopy quick detection qizhi weitong granules according to claim any one of 1-5
The method of journey, it is characterised in that
It is in the step of assay of Paeoniflorin in the detection of the water extraction process of the qizhi weitong granules (3) and/or solid
In the step of assay (3), in addition to the step of evaluate the estimated performance of the quantitative calibration model of foundation, institute
Stating evaluation index includes coefficient R, calibration set mean square deviation RMSEC, checking collection root mean square RMSEP, cross validation root mean square
RMSECV and prediction relative deviation RSEP, when R values closer to 1, RMSEC and RMSEP values it is smaller and closer to when, evaluation model
Stability is better, prediction precision is higher, then disclosure satisfy that the precision of prediction requirement of qizhi weitong granules Direct Analysis；Conversely,
Do not apply to then；
In the step of assay of aurantiin in the detection of the extraction volatile oil process of the qizhi weitong granules (3), newly
In the step of assay of aurantiamarin (3) and/or the step of determination of solid content in (3), in addition to the described quantitative of foundation
The step of estimated performance of calibrating patterns is evaluated, the evaluation index include coefficient R, calibration set mean square deviation RMSEC,
Checking collection root mean square RMSEP, cross validation root mean square RMSECV and prediction relative deviation RSEP, when R values are closer to 1, RMSEC
With RMSEP values it is smaller and closer to when, evaluation model stability is better, prediction precision is higher, then disclosure satisfy that energy-stagnation stomachache
The precision of prediction requirement of particle Direct Analysis；Conversely, not applying to then；
In the step of assay of Paeoniflorin in the detection of the extract solution concentration process of the qizhi weitong granules (3), phase
In the step of to density measurement (3) and/or the step of determination of solid content in (3), in addition to the quantitative calibration mould of foundation
The step of estimated performance of type is evaluated, the evaluation index includes coefficient R, calibration set mean square deviation RMSEC, checking collection
Root mean square RMSEP, cross validation root mean square RMSECV and prediction relative deviation RSEP, when R values closer to 1, RMSEC with
RMSEP values it is smaller and closer to when, evaluation model stability is better, prediction precision is higher, then disclosure satisfy that energy-stagnation stomachache
The precision of prediction requirement of grain Direct Analysis；Conversely, not applying to then.
7. the preparation of the utilization near infrared spectroscopy quick detection qizhi weitong granules according to claim any one of 1-6
The method of journey, it is characterised in that
In the step of assay of Paeoniflorin in the detection of the water extraction process of the qizhi weitong granules (1) and/or institute
In the step of assay of Paeoniflorin in the detection for the extract solution concentration process for stating qizhi weitong granules (1), using efficient
The paeoniflorin content of known paeoniflorin content qizhi weitong granules is used as standard content described in liquid chromatography for measuring；
In the step of determination of solid content in the detection of the water extraction process of the qizhi weitong granules (3), the energy-stagnation stomachache
In the step of determination of solid content in the detection of the extraction volatile oil process of particle (3) and/or the qizhi weitong granules is carried
In the step of taking the determination of solid content in the detection of liquid concentration process (3), the known solid content stagnation of the circulation of vital energy is determined using oven drying method
The solid content of stomachache particle is used as standard content；
In the step of assay of aurantiin in the detection of the extraction volatile oil process of the qizhi weitong granules (3), adopt
Standard content is used as with the naringin content of known naringin content qizhi weitong granules described in high effective liquid chromatography for measuring；
In the step of assay of neohesperidin in the detection of the extraction volatile oil process of the qizhi weitong granules (3),
Standard is used as using the neohesperidin content of known neohesperidin content qizhi weitong granules described in high effective liquid chromatography for measuring
Content.
8. the side of the preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules according to claim 7
Method, it is characterised in that
The tool of the paeoniflorin content of known paeoniflorin content qizhi weitong granules described in the use high effective liquid chromatography for measuring
Body step is：
(1) take the concentrated extracting solutions 4 of 4~6mL of aqueous extract or described qizhi weitong granuleses of the qizhi weitong granules~
6mL, 8~12min is centrifuged under the conditions of rotating speed 12000-14000r/min, supernatant is taken, is used as need testing solution；
(2) precision weighs 1-3mg Paeoniflorin reference substances and is placed in 20mL measuring bottles, plus methanol is made every mL and contains 0.05~0.15mg's
Solution, shakes up, and is used as reference substance solution；
(3) chromatographic condition：Using 4.6 × 250mm, 5 μm of Agilent Zorbax SB-C18 as chromatographic column, with 0.1% phosphoric acid water
Solution is mobile phase A, according to following program carry out gradient elution by Mobile phase B of acetonitrile：0-13min, A：B is 85%：15%；
13-15min, A：B is 85%：15% → 10%：90%；15-19min, A：B is 10%：90%；19-25min, A：B is
10%：90% → 0%：100%；25-30min, A：B is 0%：100% → 85%：15%；Flow velocity 1.0mL/min, column temperature 30
DEG C, Detection wavelength 230nm；
(4) it is accurate to draw the need testing solution and each 5 μ L of reference substance solution, liquid chromatograph is injected, is determined；
Using the specific step of the naringin content of known naringin content qizhi weitong granules described in high effective liquid chromatography for measuring
Suddenly it is：
(1) 4~6mL of extract solution of the extraction volatile oil process of the qizhi weitong granules is taken, in rotating speed 12000-
8~12min is centrifuged under the conditions of 14000r/min, supernatant is taken, is used as need testing solution；
(2) precision weighs 1-3mg aurantiin reference substances and is placed in 20mL measuring bottles, plus methanol is made every mL and contains 0.05~0.15mg's
Solution, shakes up, and is used as reference substance solution；
(3) chromatographic condition：Using 4.6 × 250mm, 5 μm of Agilent Zorbax SB-C18 as chromatographic column, with 0.1% phosphoric acid water
Solution is mobile phase A, according to following program carry out gradient elution by Mobile phase B of acetonitrile：0-18min, A：B is 80%：20%；
18-21min, A：B is 80%：20% → 10%：90%；21-25min, A：B is 10%：90%；21-30min, A：B is
10%：90% → 0%：100%；30-35min, A：B is 0%：100% → 80%：20%；Flow velocity 1.0mL/min, column temperature 30
DEG C, Detection wavelength 283nm；
(4) it is accurate to draw the need testing solution and each 5 μ L of reference substance solution, liquid chromatograph is injected, is determined；
Using the tool of the neohesperidin content of known neohesperidin content qizhi weitong granules described in high effective liquid chromatography for measuring
Body step is：
(1) 4~6mL of extract solution of the extraction volatile oil process of the qizhi weitong granules is taken, in rotating speed 12000-
8~12min is centrifuged under the conditions of 14000r/min, supernatant is taken, is used as need testing solution；
(2) precision weighs 1-3mg neohesperidin reference substances and is placed in 20mL measuring bottles, plus every mL is made containing 0.05~0.15mg in methanol
Solution, shake up, be used as reference substance solution；
(3) chromatographic condition：Using 4.6 × 250mm, 5 μm of Agilent Zorbax SB-C18 as chromatographic column, with 0.1% phosphoric acid water
Solution is mobile phase A, according to following program carry out gradient elution by Mobile phase B of acetonitrile：0-18min, A：B is 80%：20%；
18-21min, A：B is 80%：20% → 10%：90%；21-25min, A：B is 10%：90%；21-30min, A：B is
10%：90% → 0%：100%；30-35min, A：B is 0%：100% → 80%：20%；Flow velocity 1.0mL/min, column temperature 30
DEG C, Detection wavelength 283nm；
(4) it is accurate to draw the need testing solution and each 5 μ L of reference substance solution, liquid chromatograph is injected, is determined；
The use oven drying method determines concretely comprising the following steps for the solid content of the known solid content qizhi weitong granules：
Take the extraction volatile oil mistake of qizhi weitong granules described in the aqueous extract or 4~6mL of qizhi weitong granules described in 4~6mL
The concentrated extracting solution of qizhi weitong granules described in the extract solution or 4~6mL of journey as drying to constant weight measuring cup, in 105 DEG C
5~7h is dried, 20~40min of cooling in drier is moved to, weighs；Dry 0.5~1.5 hour, cool down at 105 DEG C, claim
Weight；Untill double difference of weighing is no more than 5mg, solid content is calculated.
9. the preparation process of the utilization near infrared spectroscopy quick detection qizhi weitong granules described in claim any one of 1-8
Purposes of the method in qizhi weitong granules quality testing and control.
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| CN110160987A (en) * | 2019-07-03 | 2019-08-23 | 温州大学 | A kind of method for quickly detecting quality of Radix Bupleuri |
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| CN113325115A (en) * | 2021-07-08 | 2021-08-31 | 辽宁华润本溪三药有限公司 | Method for establishing characteristic spectrum of qi stagnation stomachache granules and application thereof |
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