CN103163272B - Quality control method of infant spleen tonifying medicament - Google Patents
Quality control method of infant spleen tonifying medicament Download PDFInfo
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- CN103163272B CN103163272B CN201310110682.7A CN201310110682A CN103163272B CN 103163272 B CN103163272 B CN 103163272B CN 201310110682 A CN201310110682 A CN 201310110682A CN 103163272 B CN103163272 B CN 103163272B
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- Medicines Containing Plant Substances (AREA)
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Abstract
The invention discloses a quality control method of an infant spleen tonifying medicament. According to the method, hawthorn and licorice in the medicament are identified by using layer chromatography respectively, and the hesperidin content of the medicament is measured by using liquid chromatography. In the established quality control method, the medicinal material identification method is mature, feasible, high in specificity, negative and non-interfering; the content measurement method is easy to operate, high in precision and high in reproducibility; and by adopting the quality control method, the quality of the medicament can be accurately and stably controlled to adapt to industrialized stable production of the medicament.
Description
Technical field
The present invention relates to a kind of Chinese medicine for infant spleen-tonifying, particularly relate to the method for quality control of this medicine.
Background technology
Children's joins the paediatrics class medication of art Jianpi Wan system, weak for the spleen and stomach in children, and indigestion is lean and haggard, lassitude.
Children's joins the existing operative norm of art Jianpi Wan and includes in the Sanitation Ministry medicine standard Traditional Chinese medicine historical preparation the 5th.Following content has been formulated in this quality standard.
Get this product, put basis of microscopic observation: irregular branched agglomerate is colourless, meet chloral hydrate liquid and dissolve; Hyphae colorless or light brown, diameter 4-6 μm.Connection latex dust diameter 12-15 μm, containing fine particle shape thing.Pericarp lithocyte is single be dispersed in or minority in groups, lilac red, redness or yellowish-brown, similar round or polygon.The long 80-150 μm of seed coat palisade cells.Around fibrous bundle, parenchyma cell is containing calcium oxalate prismatic crystal, forms crystal fiber.
Check, relevant every regulation under pill item should be met.
Above-mentioned quality standard also exists more serious defect: first, and this standard does not carry out the quantitative measurement of active constituent content for key agents; Secondly, the composition medicine of more than 50% does not all carry out chemistry discriminating.
Chinese medicine preparation steady quality, controlled and have produce repeatability be the premise that medicine has pharmacology and clinical effectiveness repeatability, traditional Chinese medicine quality can be controlled and quality standards in Chinese drugs whether scientific, be the important restriction factor affecting industrialization of Chinese medicine.Quality controllability is the important indicator of drug assessment, and quality standard is then the imbody of drug quality controllability.
Summary of the invention
The object of this invention is to provide a kind of method of quality control of above-mentioned infant spleen-tonifying medicine, to guarantee that the drug quality of producing is stablized controlled.
The method of quality control of infant spleen-tonifying medicine provided by the invention is suitable for the medicine be prepared from by following bulk drug: Radix Codonopsis, stir-baked RHIZOMA ATRACTYLODIS MACROCEPHALAE with soil, Radix Glycyrrhizae (processed with honey), bran stir-baked SEMEN EURYALES, soil fry Semen Lablab Album, Rhizoma Dioscoreae (parched with bran), soil fry Semen Nelumbinis, dried orange peel, fry hawthorn, bran fry Medicated Leaven, fry Fructus Hordei Germinatus, Poria cocos, soil fry coix seed.Described method of quality control comprises discrimination method and content assaying method.
Wherein, described discrimination method comprises following discriminating:
1) get described medicine 10g, add zeyssatite 5g, grind well, add diethyl ether 40ml, ultrasonic process 15 minutes, filter, discard ether solution, the dregs of a decoction add ethyl acetate 40ml, ultrasonic process 15 minutes, filter, the dregs of a decoction are for subsequent use, filtrate evaporate to dryness, and residue adds methyl alcohol 2ml makes dissolving, as need testing solution; Separately get hawthorn control medicinal material 1g, with legal system for control medicinal material solution; Separately get ursolic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast; According to thin-layered chromatography test, draw need testing solution 10 μ l, control medicinal material solution 5 μ l, reference substance solution 2 μ l, puts on same silica gel g thin-layer plate, respectively with toluene: ethyl acetate: formic acid=20:4:0.5 is developping agent, launch, take out, dry, spray with 10% ethanol solution of sulfuric acid, spot development is heated to clear at 105 DEG C, in test sample chromatogram, on the position corresponding to reference substance chromatogram, aobvious identical aubergine spot;
2) get 1) in ethyl acetate extract after residue, fling to ethyl acetate, add methyl alcohol 30ml, add hot reflux 1 hour, filter, filtrate evaporate to dryness, the residue 40ml that adds water makes dissolving, extracts 3 times, each 20ml with water-saturated n-butanol, merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 3 times, each 15ml, normal butyl alcohol liquid is recycled to dry, residue adds methyl alcohol 5ml makes dissolving, as need testing solution; Another extracting Radix Glycyrrhizae control medicinal material 1g, adds methyl alcohol 20ml, is made in the same way of control medicinal material solution; According to thin-layered chromatography test, draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively on same silica gel g thin-layer plate, with methenyl choloride: acetone: formic acid=8:1:0.1 is developping agent, launch, take out, dry, spray with aluminum trichloride solution, be heated to spot development at 105 DEG C clear, inspect under putting 365nm ultraviolet lamp, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the fluorescence spot of aobvious same color.
Described content assaying method comprises the mensuration of content of hesperidin.
The present invention is specifically with the content of aurantiamarin described in following high effective liquid chromatography for measuring:
1) chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent, with methyl alcohol: water=40:60 is mobile phase; Determined wavelength 283nm; Number of theoretical plate calculates by aurantiamarin and is not less than 3000;
2) preparation of reference substance solution: get aurantiamarin reference substance appropriate, accurately weighed, add methyl alcohol and make the reference substance solution of every 1ml containing 50 μ g;
3) preparation of need testing solution: get described medicine, porphyrize, mixing, gets 0.8g, accurately weighed, add zeyssatite 0.4g, grind well, put in tool plug conical flask, precision adds methyl alcohol 25ml, close plug, weighed weight, the ultrasonic process of power 200W, frequency 40kHz 30 minutes, lets cool, weighed weight again, supplies the weight of less loss, shakes up with methyl alcohol, filter, get subsequent filtrate, to obtain final product;
4) draw reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, measures and get final product.
The present invention establishes the method for quality control of infant spleen-tonifying medicine, in the method set up, the discrimination method mature and feasible of medicinal material, specificity is strong, negative noiseless, content assaying method processing ease, precision is high, favorable reproducibility, uses method of quality control of the present invention can accurately, stably control the drug quality that children's joins art Jianpi Wan, to adapt to the industrialization steady production of medicine.
Embodiment
Embodiment 1: the TLC distinguish of hawthorn.
Get children's and join art Jianpi Wan 10g, add zeyssatite 5g, grind well, add diethyl ether 40ml, ultrasonic process 15 minutes, and filter, the dregs of a decoction add ethyl acetate 40ml, ultrasonic process 15 minutes, and filter, filtrate evaporate to dryness, residue adds methyl alcohol 2ml and dissolves, as need testing solution; With legal system for negative sample solution; Separately get hawthorn control medicinal material 1.0g, with legal system for control medicinal material solution; Separately get ursolic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast.According to thin-layered chromatography (" Chinese Pharmacopoeia " version in 2010 annex VI B) test, draw negative sample solution 10 μ l, need testing solution 10 μ l, control medicinal material solution 5 μ l, reference substance solution 2 μ l, puts respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-formic acid (20:4:0.5) for developping agent, launch, take out, dry, spray the ethanol solution of sulfuric acid with 10%, be heated to spot development at 105 DEG C clear, inspect under putting daylight.
As a result, in test sample chromatogram, on the position corresponding to reference substance and control medicinal material chromatogram, the aubergine spot of aobvious same color, on the corresponding position of negative sample chromatogram, is speckless, and illustrate negative noiseless, specificity is strong.
Embodiment 2: the TLC distinguish of Radix Glycyrrhizae.
Get children's and join art Jianpi Wan 10g, add zeyssatite 5g, grind well, add diethyl ether 40ml, ultrasonic process 15 minutes, filter, the dregs of a decoction add ethyl acetate 40ml, ultrasonic process 15 minutes, filter, the dregs of a decoction add methyl alcohol 30ml, add hot reflux 1 hour, filter, filtrate evaporate to dryness, the residue 40ml that adds water makes dissolving, extracts 3 times with normal butyl alcohol, each 20ml, merges normal butyl alcohol liquid, washes 3 times with water, evaporate to dryness, residue adds methyl alcohol 5ml makes dissolving, as need testing solution; With legal system for negative sample solution; Another extracting Radix Glycyrrhizae control medicinal material 1g, is made in the same way of control medicinal material solution.According to thin-layered chromatography (" Chinese Pharmacopoeia 2005 version annex VI B) test, draw need testing solution 10 μ l, control medicinal material solution 6 μ l, negative sample solution 10 μ l, put respectively on same silica gel g thin-layer plate, with methenyl choloride-acetone-formic acid (8:1:0.1) for developping agent, launch, take out, dry, spray, with aluminum trichloride solution, is heated to spot development at 105 DEG C clear, inspects under putting ultraviolet lamp (365nm).
In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, have three places corresponding, show identical blueness, yellow green, green fluorescence spot respectively from top to bottom, negative noiseless, specificity is strong.
Embodiment 3: the mensuration of content of hesperidin.
Children's joins art Jianpi Wan and is made up of 13 taste Chinese medicines such as Radix Codonopsis, the bighead atractylodes rhizome, Radix Glycyrrhizae, Gorgon fruit, Semen Lablab Album, Chinese yam, Semen Nelumbinis, dried orange peels, and primary standard is without assay item.In order to better control the quality of the pharmaceutical preparations and realize the monitoring of technological process, the aurantiamarin in selected dried orange peel is as assay index.
1, instrument and reagent.
Waters2695-2487 high-efficient liquid phase spectrometer, chromatographic work station (Waters, US); Aurantiamarin reference substance (lot number 0721-200010, Nat'l Pharmaceutical & Biological Products Control Institute); Methyl alcohol: chromatographically pure (α Cygni friend fine chemicals company limited); Water: pure water; It is pure that zeyssatite and other reagent are analysis.
Children's joins art Jianpi Wan.
2, chromatographic condition.
Chromatographic column: YMC-Pack ODS-A(4.6mm × 250mm); Mobile phase: methanol-water (40:60); Flow velocity: 1.0ml/min; Determined wavelength: 283nm; Column temperature: 35 DEG C.Number of theoretical plate calculates by aurantiamarin and is not less than 3000.
3, the preparation of reference substance solution.
Get aurantiamarin reference substance appropriate, accurately weighed, add methyl alcohol and make the reference substance solution of every 1ml containing 50 μ g.
4, the preparation of need testing solution.
Get children's and join art Jianpi Wan porphyrize, mixing, gets 0.8g, accurately weighed, add zeyssatite 0.4g, grind well, put in tool plug conical flask, precision adds methyl alcohol 25ml, close plug, weighed weight, ultrasonic process (power 200W, frequency 40kHz) 30 minutes, lets cool, weighed weight again, supplies the weight of less loss, shakes up with methyl alcohol, filter, get subsequent filtrate, to obtain final product.
5, the mensuration of content of hesperidin.
Accurate absorption reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
6, negative sample test.
Join art Jianpi Wan preparation prescription ratio in children's, the negative control sample of dried orange peel is removed in the preparation of simulation process method for making.Precision takes negative control sample 3g, obtains negative need testing solution by need testing solution preparation method.Under chromatographic condition, record the chromatogram of aurantiamarin reference substance, test sample and negative controls respectively, profiling results shows: in the corresponding section with aurantiamarin retention time, occur without chromatographic peak in negative controls chromatogram, namely under the condition determination determined, in preparation prescription, the mensuration of other flavour of a drug to aurantiamarin is noiseless, and method specificity is strong.
7, the investigation of linear relationship.
Get aurantiamarin reference substance storing solution (measuring bottle sealing, freezen protective, concentration 0.1002mg/ml), put to room temperature, check solution whether less loss, shake up, filter.Accurate absorption reference substance solution 2,4,6,10,15,20 μ l, each parallel sample introduction twice, measure peak area, with average peak area integrated value for ordinate, aurantiamarin reference substance sample size is that horizontal ordinate calculates regression equation, and obtaining regression equation is y=1815.7x-14240, r=0.99995, show that aurantiamarin sample size and peak area within the scope of 200.4-2004ng are good linear relationship, in table 1.
8, precision test.
Accurate absorption need testing solution, continuous sample introduction 6 times, each 10 μ l, measurement result is as table 2, and RSD is less than 3%, shows that precision is higher, and reliability is strong, and method is feasible.
9, stability test.
Get children's and join art Jianpi Wan 3g, accurately weighed, add zeyssatite 1.5g, grind well, put in 50ml tool plug conical flask, precision adds methyl alcohol 25ml, close plug, weighed weight, and ultrasonic process 1 hour, after letting cool, is supplied less loss weight with methyl alcohol, shaken up, and filters, gets subsequent filtrate.The accurate absorption need testing solution 10 μ l at 0,1,2,4,6,8 hour respectively, injection liquid chromatography, measures, the results are shown in Table 3, and need testing solution is stable in 8 hours, and RSD value is less than 3%.
10, replica test.
Get same sample lots (lot number: 081016) 0.8g, accurately weighed, extract by need testing solution preparation method respectively, assay, calculate.Result average content is 1.561mg/ml, RSD is 1.63%, the results are shown in Table 4, shows that method reappearance is good.
11, average recovery test.
Precision takes aurantiamarin reference substance 9.22mg, adds methyl alcohol and dissolves and be diluted to 100ml, shake up, and filters, makes reference substance solution, and every ml is containing aurantiamarin 0.0922mg.
Accurate absorption reference substance solution 6.5ml, puts in 50ml conical flask, evaporate to dryness, with legal system for 6 parts.Take the same batch sample 6 parts of known content (1.561mg/g), every part of about 0.4g, accurately weighed, add zeyssatite 0.2g, grind well, be transferred in conical flask, precision adds methyl alcohol 25ml respectively, close plug, weighed weight, ultrasonic process 30 minutes, lets cool, and supplies the weight of less loss with methyl alcohol, shake up, filter, get subsequent filtrate, make need testing solution.
Above-mentioned reference substance solution 5 μ l, the need testing solution 10 μ l of accurate absorption, injection liquid chromatography, measures.Calculate the recovery, result is as table 5, and the average recovery rate of aurantiamarin is 97.34%, RSD is 1.27%.
Claims (1)
1. the discrimination method of hawthorn and Radix Glycyrrhizae in an infant spleen-tonifying medicine, described infant spleen-tonifying medicine is the medicine be prepared from by following bulk drug: Radix Codonopsis, stir-baked RHIZOMA ATRACTYLODIS MACROCEPHALAE with soil, Radix Glycyrrhizae (processed with honey), bran stir-baked SEMEN EURYALES, soil fry Semen Lablab Album, Rhizoma Dioscoreae (parched with bran), soil fry Semen Nelumbinis, dried orange peel, fry hawthorn, bran fry Medicated Leaven, fry Fructus Hordei Germinatus, Poria cocos, soil fry coix seed, it is characterized in that described discrimination method comprises following discriminating:
1) get described medicine 10g, add zeyssatite 5g, grind well, add diethyl ether 40ml, ultrasonic process 15 minutes, filter, discard ether solution, the dregs of a decoction add ethyl acetate 40ml, ultrasonic process 15 minutes, filter, the dregs of a decoction are for subsequent use, filtrate evaporate to dryness, and residue adds methyl alcohol 2ml makes dissolving, as need testing solution; Separately get hawthorn control medicinal material 1g, with legal system for control medicinal material solution; Separately get ursolic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast; According to thin-layered chromatography test, draw need testing solution 10 μ l, control medicinal material solution 5 μ l, reference substance solution 2 μ l, puts on same silica gel g thin-layer plate, respectively with toluene: ethyl acetate: formic acid=20:4:0.5 is developping agent, launch, take out, dry, spray with 10% ethanol solution of sulfuric acid, spot development is heated to clear at 105 DEG C, in test sample chromatogram, on the position corresponding to reference substance chromatogram, aobvious identical aubergine spot;
2) get 1) in ethyl acetate extract after residue, fling to ethyl acetate, add methyl alcohol 30ml, add hot reflux 1 hour, filter, filtrate evaporate to dryness, the residue 40ml that adds water makes dissolving, extracts 3 times, each 20ml with water-saturated n-butanol, merge normal butyl alcohol liquid, with the saturated water washing of normal butyl alcohol 3 times, each 15ml, normal butyl alcohol liquid is recycled to dry, residue adds methyl alcohol 5ml makes dissolving, as need testing solution; Another extracting Radix Glycyrrhizae control medicinal material 1g, adds methyl alcohol 20ml, is made in the same way of control medicinal material solution; According to thin-layered chromatography test, draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively on same silica gel g thin-layer plate, with methenyl choloride: acetone: formic acid=8:1:0.1 is developping agent, launch, take out, dry, spray with aluminum trichloride solution, be heated to spot development at 105 DEG C clear, inspect under putting 365nm ultraviolet lamp, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the fluorescence spot of aobvious same color.
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