CN101606970A - The method of quality control of radix scutellariae medicinal materials - Google Patents
The method of quality control of radix scutellariae medicinal materials Download PDFInfo
- Publication number
- CN101606970A CN101606970A CNA2009100171663A CN200910017166A CN101606970A CN 101606970 A CN101606970 A CN 101606970A CN A2009100171663 A CNA2009100171663 A CN A2009100171663A CN 200910017166 A CN200910017166 A CN 200910017166A CN 101606970 A CN101606970 A CN 101606970A
- Authority
- CN
- China
- Prior art keywords
- radix scutellariae
- medicinal materials
- scutellariae medicinal
- measured
- finger printing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000463 material Substances 0.000 title claims abstract description 88
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000003908 quality control method Methods 0.000 title claims abstract description 14
- 238000007639 printing Methods 0.000 claims abstract description 52
- 238000012360 testing method Methods 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 238000005481 NMR spectroscopy Methods 0.000 claims description 20
- 238000000605 extraction Methods 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 230000005311 nuclear magnetism Effects 0.000 claims description 12
- 239000012567 medical material Substances 0.000 claims description 11
- 238000001644 13C nuclear magnetic resonance spectroscopy Methods 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 9
- 102000011759 adducin Human genes 0.000 claims description 7
- 108010076723 adducin Proteins 0.000 claims description 7
- 239000004615 ingredient Substances 0.000 claims description 7
- 238000002386 leaching Methods 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- IPQKDIRUZHOIOM-UHFFFAOYSA-N Oroxin A Natural products OC1C(O)C(O)C(CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IPQKDIRUZHOIOM-UHFFFAOYSA-N 0.000 claims description 6
- IKIIZLYTISPENI-ZFORQUDYSA-N baicalin Chemical compound O1[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IKIIZLYTISPENI-ZFORQUDYSA-N 0.000 claims description 6
- 229960003321 baicalin Drugs 0.000 claims description 6
- AQHDANHUMGXSJZ-UHFFFAOYSA-N baicalin Natural products OC1C(O)C(C(O)CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 AQHDANHUMGXSJZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001460 carbon-13 nuclear magnetic resonance spectrum Methods 0.000 claims description 6
- LKOJGSWUMISDOF-UHFFFAOYSA-N oroxylin A Chemical compound C=1C(=O)C2=C(O)C(OC)=C(O)C=C2OC=1C1=CC=CC=C1 LKOJGSWUMISDOF-UHFFFAOYSA-N 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- BJBKXYIIWYIZCX-UHFFFAOYSA-N Trigraecum Natural products C1=C(O)C(OC)=CC(C(C=2)=O)=C1OC=2C1=CC=CC=C1 BJBKXYIIWYIZCX-UHFFFAOYSA-N 0.000 claims description 3
- HIMJIPRMECETLJ-UHFFFAOYSA-N Wogonin Natural products COc1cc(O)c(O)c2C(=O)C=C(Oc12)c3ccccc3 HIMJIPRMECETLJ-UHFFFAOYSA-N 0.000 claims description 3
- XLTFNNCXVBYBSX-UHFFFAOYSA-N wogonin Chemical compound COC1=C(O)C=C(O)C(C(C=2)=O)=C1OC=2C1=CC=CC=C1 XLTFNNCXVBYBSX-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-OUBTZVSYSA-N Carbon-13 Chemical compound [13C] OKTJSMMVPCPJKN-OUBTZVSYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 10
- 239000000470 constituent Substances 0.000 abstract description 6
- 238000001228 spectrum Methods 0.000 abstract description 4
- 238000010998 test method Methods 0.000 abstract description 3
- 239000004480 active ingredient Substances 0.000 abstract description 2
- 239000003814 drug Substances 0.000 description 17
- 238000001514 detection method Methods 0.000 description 6
- 238000005160 1H NMR spectroscopy Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004811 liquid chromatography Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000013557 residual solvent Substances 0.000 description 2
- 241000007126 Codonopsis pilosula Species 0.000 description 1
- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical compound [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 description 1
- 206010013709 Drug ineffective Diseases 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229940126678 chinese medicines Drugs 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000001815 facial effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004962 physiological condition Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000425 proton nuclear magnetic resonance spectrum Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
Images
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
A kind of method of quality control of radix scutellariae medicinal materials is got the standard radix scutellariae medicinal materials, obtains its nuclear magnetic resoance spectrum, and utilizes the characteristic chemical constituent of Radix Scutellariae, points out out the characteristic peak of the characteristic peak of Radix Scutellariae active ingredient as Radix Scutellariae; Get Radix Scutellariae sample to be measured, adopt with the identical method of preparation method, test condition, method of testing of standard radix scutellariae medicinal materials and measure, obtain finger printing, the NMR fingerprint of radix scutellariae medicinal materials to be measured and the finger printing of standard radix scutellariae medicinal materials are compared.According to the difference at the characteristic resonances peak of the finger printing of radix scutellariae medicinal materials to be measured and standard radix scutellariae medicinal materials and the number of common characteristic formant, radix scutellariae medicinal materials can be divided into high-class product N>20, Grade A 18≤N≤20, goods of inferior quality 16≤N<18, certified products 14≤N<16, substandard product N<14.
Description
Technical field
The present invention relates to the method for quality control of Chinese medicine, specifically the method for quality control of radix scutellariae medicinal materials the invention still further relates to the NMR fingerprint of the resulting radix scutellariae medicinal materials of method thus.
Background technology
At present, to the evaluation of radix scutellariae medicinal materials, choose one, two active component or the index components of Radix Scutellariae often and carry out assay, and how much judge quality with its content.If only judge the inherent quality of Radix Scutellariae with the active component of one, two Radix Scutellariae, have certain one-sidedness, said nothing of the index components of no drug effect.Control the effect of radix scutellariae medicinal materials, just can not must be controlled its material group integral body, therefore need to characterize effectively on the whole Chinese medicine quality only at one, two chemical constituents.The material base of Chinese medicine is a chemical constituent, and chemical constituent method by experiment can be characterized by finger printing, and the respective substance basis can be represented in the peak of collection of illustrative plates, if material base composition faciation together, the finger printing that is showed should be consistent.At present, finger printing has become the effective means of internationally recognized control Chinese medicine or natural drug quality.Leaf just very waits (application for a patent for invention number 200610014203.1) people to propose a kind of method of quality control of codonopsis pilosula, employing be the quality of differentiating and estimate medical material by the difference of medical material reference substance liquid-phase chromatograph finger print atlas and medical material liquid-phase chromatograph finger print atlas to be measured relatively.The feasibility of finger printing discriminating Chinese crude drug quality and reliability are based on the detection method that obtains finger printing.The advantage of liquid chromatography detecting method is: liquid chromatograph has good objectivity and The better resolution, disposable Instrument purchase investment is less relatively, but this method belongs to deflection selectivity detection method is arranged, need have the property of intervention to be unfavorable in body and original position analysis sample with destructiveness; Need carry out comparatively complicated preparation and flux is limited to sample; Qualitative (structure is determined) to unknown material has suitable difficulty; The repeatability of method is general.The shortcoming of liquid chromatography detecting method is: there are certain problem in stability before and after stratographic resolution and the chromatographic column sample introduction or repeatability and the qualitative aspects such as (determining structure) of unknown material, all need to be resolved hurrily.In order to overcome the problems referred to above of liquid chromatograph, need to utilize more advanced analysis test method that more objective and accurate Chinese medicine fingerprint is provided.Utilize the NMR fingerprint control Chinese medicine quality of Chinese medicine under this background, to propose just.The advance of Chinese medicine NMR fingerprint and reliability are based on the advantage of nuclear magnetic resonance spectroscopy method of testing.The advantage of magnetic resonance spectroscopy comprises: good objectivity and repeatability, thereby be convenient to the exchange and the comparison of data between the different experiments chamber; Sample does not need loaded down with trivial details processing, can experimentize near under the physiological condition; Have non-invasively, do not destroy structures of samples and character, thereby be convenient to the detection of dynamic of live body, original position; The response coefficient of each active substance is identical in the Chinese medicine extract, therefore can carry out disposable synchronously, do not have the detection of deflection and have good in situ quantitation effect, therefore the application of nuclear magnetic resonance, NMR in the research of complex systems such as Chinese medicine at present is extensive day by day.Simultaneously NMR fingerprint can provide the numerous structural information of Chinese medicine feature extraction thing rapidly reliably, have simple to operate, reliable results, cost is low, advantages such as the many and favorable reproducibility of quantity of information.Therefore, there is strict corresponding relationship in the Chinese medicine feature extraction thing for obtaining under the identical separation program between the NMR fingerprint of Chinese medicine and the herbal species, can be used as the standard of different Chinese medicines of accurate discriminating and the true and false quality of identification Chinese medicine own.
At present to the research of botanical herbs finger printing mainly concentrate on proton nmr spectra (
1HNMR) finger printing aspect, this mainly is because of the required sample size of finger printing also seldom, sweep time is short, obtains easily, so be widely used; But because
1HNMR composes narrow distribution range, therefore causes
1HNMR spectrum fused peaks showed increased forms Bao Feng easily, thereby makes the characteristic signal be difficult to distinguish and point out.In order to overcome above shortcoming, just need to obtain its 13C-NMR (
13CNMR) finger printing, this mainly be because
13CNMR spectrum has the chemical shift range of broad, can distinguish the different carbon atoms that minute differences is structurally arranged in the molecule, and can observe not with proton directly links to each other and contain the carbon functional group, than
1HNMR can provide the structural information of more relevant carbon skeletons, simultaneously
13The probability of CNMR spectrum signal peak overlapping is less, so
13The characteristic signal ratio of CNMR
1HNMR is easier to be distinguished and points out, thereby has higher characteristic.
Summary of the invention
The objective of the invention is by to Radix Scutellariae extract
13A kind of method of Radix Scutellariae quality control is found out in the research of CNMR finger printing, sets up standard radix scutellariae medicinal materials finger printing, and as one of index of quality control and real and fake discrimination, the present invention also provides Radix Scutellariae simultaneously with the finger printing of Radix Scutellariae
13The CNMR standard finger-print.
The present invention implements a kind of method of quality control of radix scutellariae medicinal materials through the following steps, it is characterized in that comprising the steps: that (1) use superconduction pulse Fourier transform NMR spectrometer to set up the 13C-NMR finger printing of standard radix scutellariae medicinal materials and radix scutellariae medicinal materials to be measured with the carbon-13 nuclear magnetic resonance spectrum method; (2) according to the difference at the characteristic resonances peak in radix scutellariae medicinal materials to be measured and the standard radix scutellariae medicinal materials finger printing and the quantity of common characteristic formant, radix scutellariae medicinal materials to be measured can be divided into different qualities.
The described finger printing of setting up the standard radix scutellariae medicinal materials with the carbon-13 nuclear magnetic resonance spectrum method specifically comprises the steps: the preparation of (1) standard radix scutellariae medicinal materials feature extraction thing: get standard radix scutellariae medicinal materials 5g, add 95% ethanol 50mL, reflux is 2 times in water-bath, each 1 hour, the leaching extracting solution, with solvent evaporates, it is standby to obtain standard Radix Scutellariae medical material feature extraction thing;
(2) mensuration of standard radix scutellariae medicinal materials finger printing: precision takes by weighing exsiccant standard Radix Scutellariae medical material feature extraction thing 10.0mg in the nuclear-magnetism test tube, and precision is measured 0.50mL deuterated dimethyl sulfoxide (DMSO-d
6) in the nuclear-magnetism test tube, shake up, measure 25 ℃ of temperature, utilize superconduction pulse Fourier transform NMR spectrometer to obtain the 13C-NMR finger printing of standard radix scutellariae medicinal materials.
The described 13C-NMR finger printing of setting up radix scutellariae medicinal materials to be measured with the carbon-13 nuclear magnetic resonance spectrum method specifically comprises the steps: the preparation of (1) radix scutellariae medicinal materials feature extraction to be measured thing: get radix scutellariae medicinal materials 5g to be measured, add 95% ethanol 50mL, reflux is 2 times in water-bath, each 1 hour, the leaching extracting solution, with solvent evaporates, it is standby to obtain radix scutellariae medicinal materials feature extraction thing to be measured;
(2) mensuration of radix scutellariae medicinal materials finger printing to be measured: precision takes by weighing exsiccant radix scutellariae medicinal materials feature extraction thing 10.0mg to be measured in the nuclear-magnetism test tube, and precision is measured 0.50mLDMSO-d
6In the nuclear-magnetism test tube, shake up, measure 25 ℃ of temperature, utilize superconduction pulse Fourier transform NMR spectrometer to obtain the carbon-13 nmr of radix scutellariae medicinal materials to be measured.
Definite method of common characteristic formant, the common characteristic formant is that the formant of the effective ingredient that contains according to Radix Scutellariae is determined, the characteristic effective ingredient that Radix Scutellariae contains comprises baicalin, oroxylin A, wogonin and baicalin, determines the common characteristic peak of radix scutellariae medicinal materials according to the feature of the feature nuclear magnetic resonance peak of four kinds of effective ingredient in the Radix Scutellariae and finger printing thereof.
Definite method of common characteristic formant number N; There is formant in formant in the finger printing in the scope of characteristic resonances peak left and right sides 0.5ppm, think that promptly this common characteristic formant exists; Radix scutellariae medicinal materials can be divided into the medical material of different qualities, high-class product N>20, Grade A 18≤N≤20, goods of inferior quality 16≤N<18 according to common characteristic formant number N), certified products 14≤N<16, substandard product N<14.
The 13CNMR data of four kinds of characteristic effective ingredient in the table .1 Radix Scutellariae extract
??NO | Baicalin | Oroxylin A, | Wogonin | Baicalin |
??1 | ??182.5 | ??182.2 | ??182.0 | ??182.0 |
??2 | ??163.4 | ??163.2 | ??163.01 | ??163.1 |
??3 | ??153.0 | ??156.5 | ??156.3 | ??151.3 |
??4 | ??152.2 | ??152.3 | ??149.7 | ??148.7 |
??5 | ??147.0 | ??152.6 | ??156.1 | ??146.1 |
??6 | ??132.1 | ??132.2 | ??132.0 | ??131.3 |
??7 | ??131.8 | ??130.8 | ??130.7 | ??103.5 |
??8 | ??129.5 | ??129.2 | ??129.2 | ??128.5 |
??9 | ??129.1 | ??130.2 | ??99.0 | ??128.7 |
??10 | ??126.7 | ??126.4 | ??126.2 | ??125.9 |
??11 | ??105.0 | ??105.1 | ??105.2 | ??105.5 |
??12 | ??104.7 | ??104.6 | ??103.6 | ??104.2 |
??13 | ??94.6 | ??94.5 | ??127.7 | ??93.9 |
??14 | ??60.7 | ??61.0 |
The chemical shift at the total peak of table .2 Radix Scutellariae extract
Table .3 is for chemical shift and the formant number of surveying the total peak of Radix Scutellariae extract
Sequence number | The total formant position/ppm of the feature of contrast Radix Scutellariae | In generation, surveyed the formant position/ppm of Radix Scutellariae | Whether be the characteristic resonances peak |
??1 | ??182 | ??182.2 | Be |
??2 | ??163 | ??163.4 | Be |
??3 | ??157 | ??157.4 | Be |
??4 | ??154 | ??154.5 | Be |
??5 | ??153 | ??153.2 | Be |
??6 | ??152 | ??152.1 | Be |
??7 | ??151 | ??151.5 | Be |
??8 | ??150 | ??150.3 | Be |
??9 | ??149 | ??149.3 | Be |
??10 | ??146 | ??146.7 | Be |
??11 | ??132 | ??132.9 | Be |
??12 | ??131 | ??131.5 | Be |
??13 | ??130 | ??130.5 | Be |
??14 | ??129 | ??129.2 | Be |
??15 | ??128 | ??128.1 | Be |
??16 | ??126 | ??126.1 | Be |
??17 | ??105 | ??105.0 | Be |
??18 | ??103 | ??103.2 | Be |
??19 | ??99 | ??99.4 | Be |
??20 | ??95 | ??95.0 | Be |
??21 | ??93 | ??93.5 | Be |
??22 | ??61 | ??61.1 | Be |
The invention has the beneficial effects as follows:
(1) the Radix Scutellariae NMR finger printing that obtains with Radix Scutellariae extract can be represented most of active ingredient of radix scutellariae medicinal materials, can characterize the quality of radix scutellariae medicinal materials effectively.
(2) do as a wholely to treat with the finger printing of Radix Scutellariae extract, pay attention to the fingerprint characteristic peak and the mutual relation of various chemical constituents, pay attention to the whole facial feature of medical material, both avoided judging the one-sidedness of Radix Scutellariae total quality, and reduced artificial subjective judgment again and cause the probability of error because of only measuring one, two index chemical constituent.The present invention provides new reference standard for quality complete, that accurately estimate Radix Scutellariae, will contribute for improving Radix Scutellariae quality and curative effect.
(3) advantage of the present invention is based on the characteristics of magnetic resonance detection method, nuclear magnetic resonance map has unicity, comprehensive, quantitatively property and the easily characteristics of the property distinguished, the advantage that magnetic resonance detection can provide the multidimensional of reflection molecular characterization to cease characteristic signal more, make the NMR fingerprint authentication technique can provide the number of characteristics signal from many aspects, multi-angle is described the structures of samples feature, thereby makes Chinese medicine NMR fingerprint authentication technique really reach repeated height, characteristic is strong, contain much information, the scope of application is wide, identification result is advantage accurately.
Description of drawings
Fig. 1 is the finger printing of radix scutellariae medicinal materials to be measured and standard radix scutellariae medicinal materials.
The specific embodiment
Embodiment 1: the method that a kind of radix scutellariae medicinal materials finger printing is set up, and it is to take following steps:
(1) foundation of standard radix scutellariae medicinal materials finger printing
The preparation of standard radix scutellariae medicinal materials feature extraction thing:
Get standard radix scutellariae medicinal materials 5g, add 95% ethanol 50mL, reflux is 2 times in water-bath, and each 1 hour, the leaching extracting solution, with solvent evaporates, residue is standby.
The mensuration of standard radix scutellariae medicinal materials finger printing:
Precision takes by weighing 4 hours feature extraction thing 10.0mg of 60 ℃ of dryings in the nuclear-magnetism test tube, and precision is measured 0.5mLDMSO-d
6In the nuclear-magnetism test tube, shake up usefulness to be tested.Condition determination: measure 25 ℃ of temperature, scanning times is 8000 times, DMSO-d
6Make solvent, δ 39.49 residual solvent peaks are interior mark.
(2) foundation of radix scutellariae medicinal materials finger printing to be measured: get radix scutellariae medicinal materials to be measured, measure the finger printing of this Radix Scutellariae medical material to be measured according to Step By Condition described in above-mentioned (1).
(3) in described generation, surveyed the radix scutellariae medicinal materials finger printing and described standard radix scutellariae medicinal materials finger printing compares, discern the common formant that both have and the quantity of common characteristic formant, determine the quality of product quality.
Embodiment 2:(1) standard radix scutellariae medicinal materials sample characteristic extract preparation: get standard radix scutellariae medicinal materials sample 5g, add 95% ethanol 50mL, reflux is 2 times in water-bath, and each 1 hour, the leaching extracting solution, with solvent evaporates, residue is standby.
(2) standard radix scutellariae medicinal materials feature extraction thing preparation: get for test agent 5g, add 95% ethanol 50mL, reflux is 2 times in water-bath, and each 1 hour, the leaching extracting solution, with solvent evaporates, residue is standby.
(3) assay method: precision takes by weighing 4 hours various feature extraction thing 20.0mg of 60 ℃ of dryings in the nuclear-magnetism test tube, and precision is measured 0.5mLDMSO-d
6In the nuclear-magnetism test tube, shake up usefulness to be tested.Condition determination: measure 25 ℃ of temperature, scanning times is 8000 times, DMSO-d
6Make solvent, δ 39.49 residual solvent peaks are interior mark, obtain standard radix scutellariae medicinal materials finger printing.
(4) measure the finger printing of radix scutellariae medicinal materials to be measured according to above-mentioned described Step By Condition.
(5) set up standard radix scutellariae medicinal materials finger printing, the testing sample quality is judged in Radix Scutellariae sample finger printing to be measured and the contrast of standard radix scutellariae medicinal materials finger printing.Described radix scutellariae medicinal materials finger printing to be measured and described standard radix scutellariae medicinal materials finger printing are compared, and discerning the common formant that both have and the quantity of common characteristic formant is 22, and the quality of determining product is an imperial.
The finger printing of radix scutellariae medicinal materials finger printing to be measured and standard radix scutellariae medicinal materials as shown in Figure 1, the formant data as the table .3 shown in.
Claims (5)
1, a kind of method of quality control of radix scutellariae medicinal materials is characterized in that comprising the steps:
(1) use superconduction pulse Fourier transform NMR spectrometer to set up the 13C-NMR finger printing of standard radix scutellariae medicinal materials and radix scutellariae medicinal materials to be measured with the carbon-13 nuclear magnetic resonance spectrum method; (2) according to the difference at the characteristic resonances peak in radix scutellariae medicinal materials to be measured and the standard radix scutellariae medicinal materials finger printing and the quantity of common characteristic formant, radix scutellariae medicinal materials to be measured can be divided into different qualities.
2, the method for quality control of radix scutellariae medicinal materials according to claim 1, it is characterized in that the described finger printing of setting up the standard radix scutellariae medicinal materials with the carbon-13 nuclear magnetic resonance spectrum method specifically comprises the steps: the preparation of (1) standard radix scutellariae medicinal materials feature extraction thing: get standard radix scutellariae medicinal materials 5g, add 95% ethanol 50mL, reflux is 2 times in water-bath, each 1 hour, the leaching extracting solution, with solvent evaporates, it is standby to obtain standard Radix Scutellariae medical material feature extraction thing;
(2) mensuration of standard radix scutellariae medicinal materials finger printing: precision takes by weighing exsiccant standard Radix Scutellariae medical material feature extraction thing 10.0mg in the nuclear-magnetism test tube, and precision is measured 0.50mL DMSO-d
6In the nuclear-magnetism test tube, shake up, measure 25 ℃ of temperature, utilize superconduction pulse Fourier transform NMR spectrometer to obtain the 13C-NMR finger printing of standard radix scutellariae medicinal materials.
3, the method for quality control of radix scutellariae medicinal materials according to claim 1, it is characterized in that the described 13C-NMR finger printing of setting up radix scutellariae medicinal materials to be measured with the carbon-13 nuclear magnetic resonance spectrum method specifically comprises the steps: the preparation of (1) radix scutellariae medicinal materials feature extraction to be measured thing: get radix scutellariae medicinal materials 5g to be measured, add 95% ethanol 50mL, reflux is 2 times in water-bath, each 1 hour, the leaching extracting solution, with solvent evaporates, it is standby to obtain radix scutellariae medicinal materials feature extraction thing to be measured;
(2) mensuration of radix scutellariae medicinal materials finger printing to be measured: precision takes by weighing exsiccant radix scutellariae medicinal materials feature extraction thing 10.0mg to be measured in the nuclear-magnetism test tube, and precision is measured 0.50mL DMSO-d
6In the nuclear-magnetism test tube, shake up, measure 25 ℃ of temperature, utilize superconduction pulse Fourier transform NMR spectrometer to obtain the carbon-13 nmr of radix scutellariae medicinal materials to be measured.
4, the method for quality control of radix scutellariae medicinal materials according to claim 1, the definite method that it is characterized in that the common characteristic formant, the common characteristic formant is that the formant of the effective ingredient that contains according to Radix Scutellariae is determined, the characteristic effective ingredient that Radix Scutellariae contains comprises baicalin, oroxylin A, wogonin and baicalin, determines the common characteristic peak of radix scutellariae medicinal materials according to the feature of the feature nuclear magnetic resonance peak of four kinds of effective ingredient in the Radix Scutellariae and finger printing thereof.
5, the method for quality control of radix scutellariae medicinal materials according to claim 4 is characterized in that definite method of common characteristic formant number N; There is formant in formant in the finger printing in the scope of characteristic resonances peak left and right sides 0.5ppm, think that promptly this common characteristic formant exists; Radix scutellariae medicinal materials can be divided into the medical material of different qualities, high-class product N>20, Grade A 18≤N≤20, goods of inferior quality 16≤N<18, certified products 14≤N<16, substandard product N<14 according to common characteristic formant number N.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNA2009100171663A CN101606970A (en) | 2009-07-23 | 2009-07-23 | The method of quality control of radix scutellariae medicinal materials |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNA2009100171663A CN101606970A (en) | 2009-07-23 | 2009-07-23 | The method of quality control of radix scutellariae medicinal materials |
Publications (1)
Publication Number | Publication Date |
---|---|
CN101606970A true CN101606970A (en) | 2009-12-23 |
Family
ID=41480980
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNA2009100171663A Pending CN101606970A (en) | 2009-07-23 | 2009-07-23 | The method of quality control of radix scutellariae medicinal materials |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN101606970A (en) |
Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102147378A (en) * | 2011-02-28 | 2011-08-10 | 周至譓 | Method for analyzing traditional Chinese medicine dimethyl sulfoxide extracting solution by nuclear magnetic resonance technology |
CN103134827A (en) * | 2013-01-29 | 2013-06-05 | 河南省科高植物天然产物开发工程技术有限公司 | Method for identifying angled bittersweet seed medicinal materials |
CN103149232A (en) * | 2013-01-30 | 2013-06-12 | 河南省科高植物天然产物开发工程技术有限公司 | Method for identifying pyrethrum derivatives |
CN103674996A (en) * | 2012-10-24 | 2014-03-26 | 河南省科高植物天然产物开发工程技术有限公司 | Method for distinguishing salvia miltiorrhiza medicinal material or derivative |
CN103776861A (en) * | 2014-01-22 | 2014-05-07 | 瀚盟生物技术(天津)有限公司 | Method for measuring content of scutellarin in breviscapine tablet |
CN103884731A (en) * | 2013-12-28 | 2014-06-25 | 丽珠集团利民制药厂 | Nuclear magnetic resonance quality control method for ginseng and astragalus strengthening injection |
CN104181186A (en) * | 2014-09-03 | 2014-12-03 | 山西大学 | A method for constructing the 1H-NMR fingerprint of Astragalus injection |
CN104297277A (en) * | 2013-07-15 | 2015-01-21 | 天士力制药集团股份有限公司 | 1H-NMR Fingerprint of Compound Danshen Dripping Pills |
CN104880478A (en) * | 2015-05-15 | 2015-09-02 | 上海交通大学 | Method for detecting content of glycerophosphoryl choline |
CN108319810A (en) * | 2018-02-05 | 2018-07-24 | 中国药科大学 | A kind of traditional Chinese medicine quality marker finds method and Huangqin-Tang quality mark object group |
CN109507311A (en) * | 2018-10-24 | 2019-03-22 | 扬子江药业集团有限公司 | A kind of identification method of radix scutellariae and its application |
CN110441455A (en) * | 2019-04-19 | 2019-11-12 | 隆德县葆易圣药业有限公司 | A kind of method for building up of the radix scutellariae finger-print based on SFC-DAD technology and application |
-
2009
- 2009-07-23 CN CNA2009100171663A patent/CN101606970A/en active Pending
Cited By (20)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102147378A (en) * | 2011-02-28 | 2011-08-10 | 周至譓 | Method for analyzing traditional Chinese medicine dimethyl sulfoxide extracting solution by nuclear magnetic resonance technology |
CN103674996A (en) * | 2012-10-24 | 2014-03-26 | 河南省科高植物天然产物开发工程技术有限公司 | Method for distinguishing salvia miltiorrhiza medicinal material or derivative |
CN103674996B (en) * | 2012-10-24 | 2016-02-10 | 河南省科高植物天然产物开发工程技术有限公司 | A kind of method differentiating red rooted salvia or spin-off |
CN103134827B (en) * | 2013-01-29 | 2015-07-01 | 河南省科高植物天然产物开发工程技术有限公司 | Method for identifying angled bittersweet seed medicinal materials |
CN103134827A (en) * | 2013-01-29 | 2013-06-05 | 河南省科高植物天然产物开发工程技术有限公司 | Method for identifying angled bittersweet seed medicinal materials |
CN103149232A (en) * | 2013-01-30 | 2013-06-12 | 河南省科高植物天然产物开发工程技术有限公司 | Method for identifying pyrethrum derivatives |
CN104297277B (en) * | 2013-07-15 | 2018-07-06 | 天士力医药集团股份有限公司 | 1H-NMR fingerprint spectrum of compound salvia miltiorrhiza dropping pill |
CN104297277A (en) * | 2013-07-15 | 2015-01-21 | 天士力制药集团股份有限公司 | 1H-NMR Fingerprint of Compound Danshen Dripping Pills |
CN103884731A (en) * | 2013-12-28 | 2014-06-25 | 丽珠集团利民制药厂 | Nuclear magnetic resonance quality control method for ginseng and astragalus strengthening injection |
CN103884731B (en) * | 2013-12-28 | 2016-09-28 | 丽珠集团利民制药厂 | A kind of SHENQI FUZHENG ZHUSHEYE nuclear magnetic resonance, NMR method of quality control |
CN103776861B (en) * | 2014-01-22 | 2016-05-25 | 瀚盟测试科技(天津)有限公司 | A kind of method of measuring Scutellarin in Brevisapin Tablets content |
CN103776861A (en) * | 2014-01-22 | 2014-05-07 | 瀚盟生物技术(天津)有限公司 | Method for measuring content of scutellarin in breviscapine tablet |
CN104181186A (en) * | 2014-09-03 | 2014-12-03 | 山西大学 | A method for constructing the 1H-NMR fingerprint of Astragalus injection |
CN104181186B (en) * | 2014-09-03 | 2016-08-24 | 山西大学 | A Construction Method of 1H-NMR Fingerprint of Astragalus Injection |
CN104880478A (en) * | 2015-05-15 | 2015-09-02 | 上海交通大学 | Method for detecting content of glycerophosphoryl choline |
CN108319810A (en) * | 2018-02-05 | 2018-07-24 | 中国药科大学 | A kind of traditional Chinese medicine quality marker finds method and Huangqin-Tang quality mark object group |
CN108319810B (en) * | 2018-02-05 | 2020-08-04 | 中国药科大学 | Method for discovering quality marker of traditional Chinese medicine and scutellaria baicalensis decoction quality marker group |
CN109507311A (en) * | 2018-10-24 | 2019-03-22 | 扬子江药业集团有限公司 | A kind of identification method of radix scutellariae and its application |
CN110441455A (en) * | 2019-04-19 | 2019-11-12 | 隆德县葆易圣药业有限公司 | A kind of method for building up of the radix scutellariae finger-print based on SFC-DAD technology and application |
CN110441455B (en) * | 2019-04-19 | 2022-03-08 | 隆德县葆易圣药业有限公司 | Method for establishing scutellaria baicalensis fingerprint spectrum based on SFC-DAD technology and application |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101606970A (en) | The method of quality control of radix scutellariae medicinal materials | |
CN107132304B (en) | A kind of Polygala tenuifolia finger-print and index component content method for measuring | |
CN106442599B (en) | Method and device for measuring oil content of rock | |
CN106353430B (en) | Prostate capsule quality evaluation method based on multi-index active ingredient determination | |
CN109374762A (en) | A method for identification of tangerine peel and tangerine peel varieties based on metabolomics | |
CN111487347A (en) | Method for detecting fingerprint of Zhishu granules | |
CN102370891A (en) | Method for authenticating dendrobium officinale by using HPLC fingerprint | |
CN109406645A (en) | A kind of Antisathmatic oral liquid for child epheday intermedia, the detection method for frying semen armeniacae amarae, Radix Glycyrrhizae, radix scutellariae | |
CN111323491B (en) | Construction method and quality detection method of UPLC characteristic spectrum of radix Saposhnikoviae medicinal material | |
CN103115973B (en) | A method for judging batch consistency of traditional Chinese medicine | |
CN102141555A (en) | Method for establishing high-pressure liquid-phase fingerprinting of evodia and extractives thereof | |
CN115201393B (en) | Quality detection method of rhizoma polygonati and semen euryales soup | |
CN112903890A (en) | Method for identifying traditional Chinese medicine components in food based on high-resolution mass spectrometry technology | |
CN108152386B (en) | Identification method and application of tea origin in micro-region based on fingerprint technology | |
CN109507312A (en) | A kind of identification method of Cortex Phellodendri and its application | |
CN104849375A (en) | Method for detecting exocarpium citrus grandis Tanke compound | |
CN113009040A (en) | Detection method of fingerprint of strong loquat syrup and fingerprint thereof | |
CN111272905A (en) | Characteristic spectrum construction method and detection method of motherwort fruit medicinal material | |
CN112557546B (en) | Method for detecting UPLC fingerprint spectrum and multi-component content of exocarpium citri grandis pear syrup | |
CN115684382A (en) | Construction method and application of fingerprint of traditional Chinese medicinal materials of Plantago major, plantago major and mixed primordial plantain | |
CN115508492A (en) | A fingerprint construction method and fingerprint spectrum of new compound aloe vera capsules | |
CN103316073A (en) | Certified fraxinus bungeana extract product, and method for identifying certified fraxinus bungeana and its various kinds | |
CN101904952A (en) | Quality evaluation method of alisma extract | |
Wang et al. | A high-performance liquid chromatography method for quality control of complex substances: analysis of marker alkaloids and flavonoids of the herb Herba leonuri (Yimucao) | |
CN107976494B (en) | Construction of standard characteristic spectrum of Kangfu tincture and quality detection method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20091223 |