CN102028859B - Detection method for Chinese medicinal preparation for treating asthma - Google Patents
Detection method for Chinese medicinal preparation for treating asthma Download PDFInfo
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- CN102028859B CN102028859B CN200910070660.6A CN200910070660A CN102028859B CN 102028859 B CN102028859 B CN 102028859B CN 200910070660 A CN200910070660 A CN 200910070660A CN 102028859 B CN102028859 B CN 102028859B
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Abstract
The invention relates to a quality control method for all-flower anti-asthma pills serving as a Chinese medicinal preparation for treating asthma. The method comprises the following steps of: (1) identifying character; (2) identifying tangerine peel by thin layer chromatography; (3) identifying tree peony bark by the thin layer chromatography; (4) identifying baical skullcap root by the thin layer chromatography; (5) identifying bitter apricot seed by the thin layer chromatography; and (6) measuring ephedra herb by high performance liquid chromatography. In the detection method, on the basis of the original standard of the first book of traditional Chinese medicine preparations in set prescriptions which accord with medicament standard of ministry of health, reference medicinal materials and thin layer identification and detection methods of reference substances are added, and a method for measuring content by the high performance liquid chromatography is drawn; and by the amended quality standard control method, the controllability of the quality standard of the all-flower anti-asthma pills is improved, the intrinsic quality and the curative effect of a product are further guaranteed, and the quality control method has great significance to promotion of product sale, increase of market competitiveness of the product and guarantee of medication safety of patients.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicines, relate to the detection method of Chinese medicine, especially a kind of method of quality control for the treatment of the Chinese medicine preparation Baihuadingchuan Pill of asthma.
Background technology
Baihuadingchuan Pill is made up of ten seven to ten eight taste Chinese medicines such as tussilago, dried orange peel, the tuber of dwarf lilyturf, root of Chinese trichosanthes, moutan bark, semen armeniacae amarae, the root of large-flowered skullcap, Chinese ephedra, asters, its preparation method is for be broken into fine powder by above-mentioned each taste traditional Chinese medicine powder, to sieve, to mix, refined honey 120 ~ 130g is added at every 100g powder, make large honeyed bolus, to obtain final product.Baihuadingchuan Pill has clearing heat and eliminating phlegm, effect of relieving cough and relieving asthma, and be usually used in treatment phlegm heat and cough and breathe heavily, expiratory dyspnea, fullness sensation in chest is smooth, and the diseases such as dry throat and mouth are disease class non-prescribed medicine medicine of roaring.
Baihuadingchuan Pill with cure holy Zhang Zhongjing create " Ma Xing Shi Gan Tang " for basic prescription, the folk remedy that utilization traditional Chinese medicine theory and for many years clinical experience develop in conjunction with diagnosis and treatment based on an overall analysis of the illness and the patient's condition, has remarkable efficacy for the breathing problem such as cough, many phlegm, flu, asthma, bronchitis.This product was the private enterprise and produces before nineteen fifty-three, the Tianjin intrinsic one-tenth side unification that nineteen fifty-three includes the examination & verification of Tianjin health bureau in joins this, after this Chinese traditional patent formulation selected workss in 1956 appraised and decided in Tianjin health bureau are recorded, version in 1964 versions in 1978 and " Chinese patent drug specification ", nineteen ninety version " the Tianjin drug standards ", all give in " Drug Standard of Ministry of Public Health of the Peoples Republic of China Traditional Chinese medicine historical preparation first " (standard No.: WS3-B-0062-89) and recording, wherein Tianjin Zhongxin Pharmaceutical Group Co is one of manufacturer of Baihuadingchuan Pill.
Along with the development of economy, Chinese medicine is subject to common people and more understands and attract attention, Chinese medicine grows up under traditional instruction of Chinese Medicine theory, mostly raw material is the natural materials such as bark and grass roots, mineral, animal, wide material sources, complicated component, makes Chinese native medicine security etalon have specific characteristics, and safety standards problem becomes the difficult problem that Chinese medicine enters international market too.Although there is no the international standard of plant medicine at present in the world, the trend of Chinese medicine standard but the south east asia of the U.S., European Union, China and conventional outlet Chinese medicine is improved, in the case, need the standard proposing to be applicable to China's product quality to adapt to international standard, China has the Chinese medicine of thousands of years to use history, many Chinese medicine standards with reference to China in corresponding botanical drug product quality standard are being worked out in countries in the world, so quality standard that is perfect, that improve Chinese medicine is more extremely urgent.
Thin-layered chromatography (TLC) differentiate in the determination of control medicinal material be more and more used in Chinese medicine preparation, due to restriction or the reason such as select reference substance exclusive not of reference substance, often select the chromatographic control product that control medicinal material is differentiated as TLC.
High performance liquid chromatography (HPLC) has quick, sensitive, separation efficiency advantages of higher, in Chinese traditional medicine identification, after adopting HPLC method separation characteristic composition, carrying out structure analysis and quantitative test with UV-detector (UV) or mass detector (MS), is the effective ways of thoroughly evaluating quality.Just there are 59 kinds of medicinal materials and 50 kinds of Chinese patent drugs to adopt HPLC method to identify in Chinese Pharmacopoeia (version in 2000), but also constantly have people to identify with the Chinese medicine of HPLC method to other and constituent analysis research.
The existing quality standard statement of Baihuadingchuan Pill: " get this product and put basis of microscopic observation: pollen granule is spherical, diameter about to 32 μm, outer wall tool stings, sharper.Connection latex dust diameter 14 ~ 25 μm, containing yellow particle shape thing; Seed coat epidermis lithocyte is fallow, and surface is seen in class polygon, and wall is thicker, and hole ditch is fine and closely woven, and cell is containing burgundy thing; Glandular scale head 8 cell, oblate spheroid, diameter about to 90 μm, handle is unicellular; Pore is special, and guard cell side is seen in dumb-bell shape; Irregular flaky crystal is colourless, has straight texture.”。Above-mentioned standard obvious very fuzzy and not enough for the method for quality control of this kind, the description of part Chinese medicine microscopical characters feature is only had in original standard, for quality control standard, be nowhere near, there is no the assay item of the discriminating of feature medicinal material and the index components of reflection medicine inherent quality, effectively cannot ensure the inherent quality of product aborning, drug effect also can not be guaranteed.
According to the retrieval, at present not about the Patents of the treatment asthma class Chinese medicine particularly method of quality control of Baihuadingchuan Pill, in the important formula that existing patent mainly concentrates on treatment asthma and method.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, there is provided a kind of can the method for quality control of Chinese medicine preparation Baihuadingchuan Pill for the treatment of asthma of qualitative and quantitative analysis drug ingedient, this method has that detection means is simple, testing result feature accurately.
The object of the invention is to be achieved through the following technical solutions:
Treat a method of quality control for the Chinese medicine preparation Baihuadingchuan Pill of asthma, step is:
(1) proterties is differentiated;
(2) differentiate dried orange peel: adopting thin-layered chromatography, take aurantiamarin as reference substance, differentiate in Baihuadingchuan Pill prescription whether containing dried orange peel composition;
(3) differentiate moutan bark: adopting thin-layered chromatography, take Paeonol as reference substance, whether differentiate in Baihuadingchuan Pill prescription containing moutan bark composition;
(4) differentiate the root of large-flowered skullcap: adopting thin-layered chromatography, take scutelloside as reference substance, whether differentiate in Baihuadingchuan Pill prescription containing ingredients of Scutellaria;
(5) differentiate semen armeniacae amarae: adopting thin-layered chromatography, take semen armeniacae amarae as control medicinal material, whether differentiate in Baihuadingchuan Pill prescription containing semen armeniacae amarae composition;
(6) Chinese ephedra is measured: adopting the Chinese ephedra content in Syrups by HPLC prescription Baihuadingchuan Pill, take ephedrine hydrochloride as reference substance.
And the step that described proterties is differentiated is: character description is: Baihuadingchuan Pill is the large honeyed bolus of sepia to pitchy; Sweet, the micro-hardship of taste, puts basis of microscopic observation: pollen granule is spherical, diameter 30-35 μm, and outer wall tool stings, sharper, connection latex dust diameter 14 ~ 25 μm, containing yellow particle shape thing, seed coat epidermis lithocyte is fallow, surface is seen in class polygon, and wall is thicker, and hole ditch is fine and closely woven, cell contains burgundy thing, glandular scale head 8 cell, oblate spheroid, diameter 85-90 μm, handle is unicellular, and pore is special, guard cell side is seen in dumb-bell shape, and irregular flaky crystal is colourless, has straight texture.
And described thin-layered chromatography differentiates that the method for dried orange peel is:
1. Baihuadingchuan Pill is made need testing solution;
2. getting aurantiamarin is reference substance, adds Methanol and becomes reference substance solution;
3. the preparation of negative control solution;
4. thin-layer chromatography detect: get 1., 2., 3. solution on same silica gel thin-layer plate, with volume ratio methenyl choloride: methyl alcohol: butanone: glacial acetic acid=13: 4: 1: 1 for developping agent expansion, spray with aluminium choride test solution, be heated to spot development clear;
Whether 5. interpretation of result: inspect under thin layer plate being put ultraviolet lamp 365nm wavelength, determine in test sample containing dried orange peel composition.
And described thin-layered chromatography differentiates that the method for moutan bark is:
1. Baihuadingchuan Pill is made need testing solution;
2. getting Paeonol is reference substance, adds acetone and makes reference substance solution;
3. the preparation of negative control solution;
4. thin layer detect: get 1., 2., 3. solution on same silica gel thin-layer plate, with volume ratio cyclohexane: ethyl acetate=3: 1 for developping agent launch, spray with hydrochloric acid acidity 5% ferric trichloride ethanolic solution, be heated to spot development clear;
Whether 5. interpretation of result: the position analyzing the spot of same color on silica gel thin-layer plate, determine in test sample containing moutan bark composition.
And described thin-layered chromatography differentiates that the method for the root of large-flowered skullcap is:
1. get the dregs of a decoction be left after moutan bark is differentiated and make need testing solution;
2. getting scutelloside is reference substance, adds Methanol and becomes reference substance solution;
3. the preparation of negative control solution;
4. thin layer detect: get 1., 2., 3. solution on same silica gel thin-layer plate, with volume ratio ethyl acetate: butanone: acetic acid: water=5: 3: 1: 1 for developping agent expansion, spray with 1% ferric trichloride ethanolic solution;
Whether 5. interpretation of result: the position analyzing the spot of same color on silica gel thin-layer plate, determine in test sample containing ingredients of Scutellaria.
And described thin-layered chromatography differentiates that amygdalate method is:
1. get the dregs of a decoction be left after the root of large-flowered skullcap is differentiated and make need testing solution;
2. get semen armeniacae amarae control medicinal material, add Methanol and become control medicinal material solution;
3. the preparation of negative control solution;
4. thin layer detect: get 1., 2., 3. solution on same silica gel thin-layer plate, with volume ratio toluene: ethyl formate: methyl alcohol: formic acid: water=12: the upper solution of 4: 0.8: 0.2: 2 is that developping agent launches, spray is with volume ratio 1% (v/v) vanillic aldehyde ethanol and 3% (v/v) perchloric acid=1: 1 mixed solution, is heated to spot development clear;
Whether 5. interpretation of result: the position analyzing the spot of same color on silica gel thin-layer plate, determine in test sample containing semen armeniacae amarae composition.
And the method for described Syrups by HPLC Chinese ephedra is:
1. the setting of liquid phase chromatogram condition;
2. the preparation of standard solution;
3. the preparation of need testing solution;
4. the preparation of negative sample solution;
5. Chinese ephedra chromatogram is measured;
6. interpretation of result: the content calculating Baihuadingchuan Pill epheday intermedia according to chromatogram.
Advantage of the present invention and good effect are:
1, detection method of the present invention is on the basis of " the Sanitation Ministry medicine standard " Traditional Chinese medicine historical preparation first primary standard, add the TLC distinguish method of inspection of control medicinal material and reference substance, formulate the method that high performance liquid chromatography carries out assay, revised quality standard control method, improve the controllability of Baihuadingchuan Pill quality standard, guarantee product inherent quality and curative effect further, to promotion production marketing, the increase competitiveness of product in market, ensure that patient medication security implications is great.
2, the present invention has carried out raising, perfect to the quality standard of Baihuadingchuan Pill, on primary standard basis, add dried orange peel in prescription, moutan bark, the root of large-flowered skullcap and the amygdalate TLC distinguish method of inspection, take ephedrine hydrochloride as reference substance, formulate the method for the content adopting high effective liquid chromatography for measuring prescription epheday intermedia, revised quality standard control method is more conducive to the quality control of Chinese medicine preparation, can check out counterfeit drug and substandard drug more exactly, going abroad to the modernization of Chinese medicine and Chinese medicine is significant.
Accompanying drawing explanation
Fig. 1 is that in test sample of the present invention, dried orange peel inspects figure under wavelength is 365nm ultraviolet lamp, wherein, in Fig. 1, band is followed successively by from left to right: 1. need testing solution 1 (lot number: F624001), 2. need testing solution 2 (lot number: E624001), 3. need testing solution 3 (lot number: E573001), 4. aurantiamarin reference substance (middle inspection institute, lot number: 110721-200512), 5. dried orange peel negative sample;
Fig. 2 be in test sample of the present invention moutan bark in the sunlight inspect figure, wherein, in Fig. 2, band is followed successively by from left to right: 1. need testing solution 1 (lot number: F624001), 2. need testing solution 2 (lot number: E624001), 3. need testing solution 3 (lot number: E573001), 4. Paeonol reference substance (middle inspection institute, lot number: 11525-200404), 5. moutan bark negative sample;
In Fig. 3 test sample of the present invention the root of large-flowered skullcap in the sunlight inspect figure, wherein, in Fig. 3, band is followed successively by from left to right: 1. need testing solution 1 (lot number: F624001), 2. need testing solution 2 (lot number: E624001), 3. need testing solution 3 (lot number: E573001), 4. scutelloside reference substance (middle inspection institute, lot number: 120927-200512), 5. root of large-flowered skullcap negative sample;
Fig. 4 be in test sample of the present invention semen armeniacae amarae in the sunlight inspect figure, wherein, in Fig. 4, band is followed successively by from left to right: 1. need testing solution 1 (lot number: F624001), 2. need testing solution 2 (lot number: E624001), 3. need testing solution 3 (lot number: E573001), 4. semen armeniacae amarae control medicinal material (middle inspection institute, lot number: 121554-200601), 5. semen armeniacae amarae negative sample;
Fig. 5 is the liquid chromatogram that the present invention analyzes ephedrine hydrochloride and pseudoephedrine hydrochloride, wherein, has the peak of sign to be followed successively by from left to right: 1. ephedrine hydrochloride, 2. pseudoephedrine hydrochloride in Fig. 5;
Fig. 6 is the liquid chromatogram of ephedrine hydrochloride reference substance of the present invention (middle inspection institute, lot number: 171237-200304);
Fig. 7 is the liquid chromatogram of test sample of the present invention;
Fig. 8 is the liquid form and aspect collection of illustrative plates of Chinese ephedra negative sample of the present invention;
Fig. 9 is the liquid chromatogram that the present invention uses solvent (hydrochloric acid-methanol).
Embodiment
Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Treat a method of quality control for the Chinese medicine preparation Baihuadingchuan Pill of asthma, the step of its method is:
(1) proterties is differentiated:
Character description is: Baihuadingchuan Pill is the large honeyed bolus of sepia to pitchy; Sweet, the micro-hardship of taste.Put basis of microscopic observation: pollen granule is spherical, diameter about to 32 μm, outer wall tool stings, sharper (tussilago).Connection latex dust diameter 14 ~ 25 μm, containing yellow particle shape thing (balloonflower root).Seed coat epidermis lithocyte is fallow, and surface is seen in class polygon, and wall is thicker, and hole ditch is fine and closely woven, and cell is containing burgundy thing (fruit of Chinese magnoliavine).Glandular scale head 8 cell, oblate spheroid, diameter about to 90 μm, handle unicellular (peppermint).Pore is special, and guard cell sees into side dumb-bell shape (Chinese ephedra).Irregular flaky crystal is colourless, has straight texture (gypsum).
(2) thin-layered chromatography differentiates dried orange peel: adopting thin-layered chromatography, take aurantiamarin as reference substance, differentiates the dried orange peel in Baihuadingchuan Pill prescription.
1. the preparation of need testing solution: get Baihuadingchuan Pill 9g, shred, adds methyl alcohol 25ml, add hot reflux 30 minutes, filter, filtrate evaporate to dryness, the residue 10ml that adds water makes dissolving, 2 times are extracted with ethyl acetate jolting, each 20ml, combined ethyl acetate extract, evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, as need testing solution.
2. the preparation of reference substance solution: get aurantiamarin reference substance, adds methyl alcohol and makes saturated solution, in contrast product solution.
3. the preparation of negative sample solution: by prescription proportioning, get other flavour of a drug except dried orange peel, make pill according to the technique under [method for making] item in " the Sanitation Ministry medicine standard " Traditional Chinese medicine historical preparation first primary standard, then obtain negative sample solution by above-mentioned need testing solution preparation method.
4. thin layer detects: photograph thin-layered chromatography (" Chinese Pharmacopoeia 2005 version annex VI B) test, draw each 4 ~ 6 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with volume ratio methenyl choloride: methyl alcohol: butanone: glacial acetic acid=13: be developping agent at 4: 1: 1, launch, take out, dry, spray with aluminium choride test solution.
5. interpretation of result: the testing result of different production batch Baihuadingchuan Pill test sample is shown in Fig. 1.Inspect under putting ultraviolet lamp (365nm), in test sample chromatogram, on the position corresponding to aurantiamarin reference substance chromatogram, the fluorescence spot of aobvious same color, negative sample is also noiseless.Show that test sample contains dried orange peel composition.
(3) thin-layered chromatography differentiates moutan bark: adopting thin-layered chromatography, take Paeonol as reference substance, differentiates moutan bark in Baihuadingchuan Pill prescription.
1. the preparation of need testing solution: get Baihuadingchuan Pill 2 ball, shred, add zeyssatite 8g, grind well, add diethyl ether 40ml, adds hot reflux 60 minutes, and filter, residue is for subsequent use; Filtrate volatilizes, and residue adds acetone 1ml makes dissolving, as need testing solution.
2. the preparation of reference substance solution: get Paeonol reference substance, adds acetone and makes the solution of every 1ml containing 1mg, product solution in contrast.
3. the preparation of negative sample solution: by prescription proportioning, get other flavour of a drug except moutan bark, make pill according to the technique under [method for making] item in " the Sanitation Ministry medicine standard " Traditional Chinese medicine historical preparation first primary standard, then obtain negative sample solution by above-mentioned need testing solution preparation method.
4. thin layer detects: photograph thin-layered chromatography (" Chinese Pharmacopoeia 2005 version annex VI B) test, draw each 2 ~ 6 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with volume ratio cyclohexane: ethyl acetate=3: 1 is developping agent, launch, take out, dry, spray with the acid 5% ferric trichloride ethanolic solution of hydrochloric acid, be heated to spot development clear.
5. interpretation of result: the testing result of different production batch Baihuadingchuan Pill test sample is shown in Fig. 2.In test sample chromatogram, on the position corresponding to Paeonol reference substance chromatogram, the spot of aobvious same color, negative sample is noiseless.Show that test sample contains tree peony product composition.
(4) thin-layered chromatography differentiates the root of large-flowered skullcap: adopting thin-layered chromatography, take scutelloside as reference substance, differentiates the root of large-flowered skullcap in Baihuadingchuan Pill prescription.
1. the preparation of need testing solution: get the filter residue under the preparation of need testing solution in the discriminating of above-mentioned moutan bark, add methyl alcohol 30ml, add hot reflux 30 minutes, filter, filtrate evaporate to dryness, residue adds methyl alcohol 3ml makes dissolving, gets supernatant as need testing solution.
2. the preparation of reference substance solution: get scutelloside reference substance, adds methyl alcohol and makes the solution of every 1ml containing 1mg, product solution in contrast.
3. the preparation of negative sample solution: by prescription proportioning, get other flavour of a drug except the root of large-flowered skullcap, make pill according to the technique under [method for making] item in " the Sanitation Ministry medicine standard " Traditional Chinese medicine historical preparation first primary standard, then obtain negative sample solution by above-mentioned need testing solution preparation method.
4. thin layer detects: photograph thin-layered chromatography (" Chinese Pharmacopoeia 2005 version annex VI B) test, draw each 4 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with volume ratio ethyl acetate: butanone: formic acid: water=5: be developping agent at 3: 1: 1, launch, take out, dry, spray with 1% ferric trichloride ethanolic solution.
5. interpretation of result: the testing result of different production batch Baihuadingchuan Pill test sample is shown in Fig. 3.In test sample chromatogram, on the position corresponding to scutelloside reference substance chromatogram, the spot of aobvious same color, negative sample is noiseless.Show that test sample contains ingredients of Scutellaria.
(5) thin-layered chromatography differentiates semen armeniacae amarae: adopting thin-layered chromatography, take semen armeniacae amarae as control medicinal material, differentiates semen armeniacae amarae in Baihuadingchuan Pill prescription.
1. the preparation of need testing solution: get the need testing solution under above-mentioned root of large-flowered skullcap discriminating item.
2. the preparation of control medicinal material solution: get semen armeniacae amarae control medicinal material 1g, add methyl alcohol 15ml, adds hot reflux 30 minutes, lets cool, and filter, filtrate is medicinal material solution in contrast.
3. the preparation of negative sample solution: by prescription proportioning, get other flavour of a drug except semen armeniacae amarae, make pill according to the technique under [method for making] item in " the Sanitation Ministry medicine standard " Traditional Chinese medicine historical preparation first primary standard, then obtain negative sample solution by above-mentioned need testing solution preparation method.
4. thin layer detects: photograph thin-layered chromatography (" Chinese Pharmacopoeia 2005 version annex VI B) test, draw each 4 ~ 6 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with volume ratio toluene: ethyl formate: methyl alcohol: formic acid: water=12: the upper solution of 4: 0.8: 0.2: 2 is developping agent, launch, take out, dry, spray, with 1% vanillic aldehyde ethanol and 3% perchloric acid (1: 1) mixed solution, is heated to spot development clear.
5. interpretation of result: the testing result of different production batch Baihuadingchuan Pill test sample is shown in Fig. 4.In test sample chromatogram, on the position corresponding to semen armeniacae amarae control medicinal material chromatogram, the spot of aobvious same color, negative sample is noiseless.Show that test sample contains semen armeniacae amarae composition.
(6) Syrups by HPLC Chinese ephedra: adopting the Chinese ephedra in Syrups by HPLC prescription Baihuadingchuan Pill, take ephedrine hydrochloride as reference substance.
1. the setting of liquid phase chromatogram condition: with reference to " in Chinese Pharmacopoeia 2005 version one, " tongxuan lifei pills " content assaying method is formulated.Be filling agent with octadecylsilane chemically bonded silica; Mobile phase: second eyeball: 0.1% phosphoric acid solution=30: 870; Determined wavelength is 210nm, column temperature: 40 DEG C; Flow velocity: 1ml/ minute.Number of theoretical plate calculates by ephedrine hydrochloride peak and is not less than 5000.Adopt above-mentioned chromatographic condition, analyze, result to ephedrine hydrochloride and pseudoephedrine hydrochloride, adopt above-mentioned chromatographic condition, both can reach baseline separation.Liquid chromatographic detection the results are shown in Figure 5.
2. the preparation of standard solution: get ephedrine hydrochloride reference substance appropriate, accurately weighed, add methyl alcohol and make the solution of every 1ml containing 60 μ g, to obtain final product.Liquid chromatographic detection the results are shown in Figure 6.
3. the preparation of need testing solution: it is appropriate to get this product, shred, get about 2g, accurately weighed, add zeyssatite 2g, grind well, put in apparatus,Soxhlet's, add strong ammonia solution 3ml, with ethanol 10ml gradation washing mortar etc., be transferred in the lump and put in apparatus,Soxhlet's, then it is appropriate to add diethyl ether, heating is back to extracting liquid colourless, extract decompression is steamed near dry, residue adds methanol hydrochloride solution (1 → 1000) makes dissolving, is transferred in 10ml measuring bottle, and is diluted to scale, shake up, filter, get subsequent filtrate, to obtain final product.Liquid chromatographic detection the results are shown in Figure 7.
This method is with reference to " in Chinese Pharmacopoeia 2005 version one, " tongxuan lifei pills " content assaying method is formulated.In need testing solution preparation, according to the architectural characteristic of ephedrine hydrochloride composition, adopt surname extraction mode, liquor ammoniae fortis alkalizes, and ether makes Extraction solvent, is using extracting liquid colourless as extraction terminal.Shift incomplete phenomenon in view of in the preparation of " tongxuan lifei pills " need testing solution, using the washing lotion of the ethanol of use as instruments such as cleaning mortars, be incorporated in apparatus,Soxhlet's.Separately contain the not volatile solvents such as a small amount of ethanol in view of in extract, in view of ephedrine is secondary amine constituents, the volatile feature of tool, adopts low-temperature reduced-pressure to steam to the nearly mode done, makes need testing solution preparation method be tending towards reasonable.
4. the preparation of negative sample solution: the ingredients removing Chinese ephedra by prescription, by [method for making] in " the Sanitation Ministry medicine standard " Traditional Chinese medicine historical preparation first primary standard obtained sample, again by above-mentioned need testing solution preparation method, obtained negative sample solution, liquid chromatographic detection the results are shown in Figure (8).The liquid chromatogram (9) of another attached use solvent.
5. measure: accurate absorption reference substance solution, need testing solution, negative sample solution and each 10 μ l of use solvent respectively, injection liquid chromatography, measures, to obtain final product.
6. interpretation of result: can be determined in test sample containing ephedrine hydrochloride by retention time.With reference to " under Chinese Pharmacopoeia 2005 version Chinese ephedra item, content limit calculates, and the hydrochloric ephedrine of every g sample should be 0.29mg.Can calculate the content obtaining ephedrine hydrochloride in Baihuadingchuan Pill according to chromatogram, this content and state-promulgated pharmacopoeia compare, and can judge that whether the Chinese ephedra content of test sample is qualified, and then judge the quality of Baihuadingchuan Pill of different manufacturers, different batches.In this laboratory sample Baihuadingchuan Pill prescription, Chinese ephedra accounts for 6.7% of prescription total amount, adds refined honey 130g calculate in preparation by every 100g fecula, and every g sample is about containing Chinese ephedra fecula 29.13mg.In view of Baihuadingchuan Pill is starch, according to Chinese Pharmacopoeia Commission's requirement, starch calculates content limit by 80% rate of transform and formulates as every g contains Chinese ephedra with ephedrine hydrochloride (C
10h
15nO.HCl) count, must not 0.20mg be less than; If calculate by every ball, limit is ordered as every ball contains Chinese ephedra with ephedrine hydrochloride (C
10h
15nO.HCl) count, must not 1.8mg be less than.
Claims (1)
1. treat a detection method for the Chinese medicine preparation Baihuadingchuan Pill of asthma, the step of its method is:
(1) proterties is differentiated:
Character description is: Baihuadingchuan Pill is the large honeyed bolus of sepia to pitchy; Sweet, the micro-hardship of taste; Put basis of microscopic observation: tussilago: pollen granule is spherical, diameter about to 32 μm, outer wall tool stings, sharper; Balloonflower root: connection latex dust diameter 14 ~ 25 μm, containing yellow particle shape thing; The fruit of Chinese magnoliavine: seed coat epidermis lithocyte is fallow, surface is seen in class polygon, and wall is thicker, and hole ditch is fine and closely woven, and cell is containing burgundy thing; Peppermint: glandular scale head 8 cell, oblate spheroid, diameter about to 90 μm, handle is unicellular; Chinese ephedra: pore is special, guard cell sees into dumb-bell shape in side; Gypsum: irregular flaky crystal is colourless, has straight texture;
(2) thin-layered chromatography differentiates dried orange peel: adopting thin-layered chromatography, take aurantiamarin as reference substance, differentiates the dried orange peel in Baihuadingchuan Pill prescription;
1. the preparation of need testing solution: get Baihuadingchuan Pill 9g, shred, adds methyl alcohol 25ml, add hot reflux 30 minutes, filter, filtrate evaporate to dryness, the residue 10ml that adds water makes dissolving, 2 times are extracted with ethyl acetate jolting, each 20ml, combined ethyl acetate extract, evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, as need testing solution;
2. the preparation of reference substance solution: get aurantiamarin reference substance, adds methyl alcohol and makes saturated solution, in contrast product solution;
3. the preparation of negative sample solution: by prescription proportioning, get other flavour of a drug except dried orange peel, make pill according to the technique under [method for making] item in " Drug Standard of Ministry of Public Health of the Peoples Republic of China Traditional Chinese medicine historical preparation first " primary standard, then obtain negative sample solution by above-mentioned need testing solution preparation method;
4. thin layer detects: according to " Chinese Pharmacopoeia 2005 version annex VIB thin-layered chromatography test, draw each 4 ~ 6 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with methenyl choloride-methyl alcohol-butanone-glacial acetic acid=13: 4: 1: 1 for developping agent, launch, take out, dry, spray with aluminium choride test solution;
5. interpretation of result: the testing result of different production batch Baihuadingchuan Pill test sample; Inspect under putting ultraviolet lamp 365nm, in test sample chromatogram, on the position corresponding to aurantiamarin reference substance chromatogram, the fluorescence spot of aobvious same color, negative sample is also noiseless; Show that test sample contains dried orange peel composition;
(3) thin-layered chromatography differentiates moutan bark: adopting thin-layered chromatography, take Paeonol as reference substance, differentiates moutan bark in Baihuadingchuan Pill prescription;
1. the preparation of need testing solution: get Baihuadingchuan Pill 2 ball, shred, add zeyssatite 8g, grind well, add diethyl ether 40ml, adds hot reflux 60 minutes, and filter, residue is for subsequent use; Filtrate volatilizes, and residue adds acetone 1ml makes dissolving, as need testing solution;
2. the preparation of reference substance solution: get Paeonol reference substance, adds acetone and makes the solution of every 1ml containing 1mg, product solution in contrast;
3. the preparation of negative sample solution: by prescription proportioning, get other flavour of a drug except moutan bark, make pill according to the technique under [method for making] item in " Drug Standard of Ministry of Public Health of the Peoples Republic of China Traditional Chinese medicine historical preparation first " primary standard, then obtain negative sample solution by above-mentioned need testing solution preparation method;
4. thin layer detects: according to " Chinese Pharmacopoeia 2005 version annex VIB thin-layered chromatography test, draw each 2 ~ 6 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate=3: 1 is developping agent, launch, take out, dry, spray with the acid 5% ferric trichloride ethanolic solution of hydrochloric acid, be heated to spot development clear;
5. interpretation of result: the testing result of different production batch Baihuadingchuan Pill test sample; In test sample chromatogram, on the position corresponding to Paeonol reference substance chromatogram, the spot of aobvious same color, negative sample is noiseless; Show that test sample contains moutan bark composition;
(4) thin-layered chromatography differentiates the root of large-flowered skullcap: adopting thin-layered chromatography, take scutelloside as reference substance, differentiates the root of large-flowered skullcap in Baihuadingchuan Pill prescription;
1. the preparation of need testing solution: get the filter residue under the preparation of need testing solution in the discriminating of above-mentioned moutan bark, add methyl alcohol 30ml, add hot reflux 30 minutes, filter, filtrate evaporate to dryness, residue adds methyl alcohol 3ml makes dissolving, gets supernatant as need testing solution;
2. the preparation of reference substance solution: get scutelloside reference substance, adds methyl alcohol and makes the solution of every 1ml containing 1mg, product solution in contrast;
3. the preparation of negative sample solution: by prescription proportioning, get other flavour of a drug except the root of large-flowered skullcap, make pill according to the technique under [method for making] item in " Drug Standard of Ministry of Public Health of the Peoples Republic of China Traditional Chinese medicine historical preparation first " primary standard, then obtain negative sample solution by above-mentioned need testing solution preparation method;
4. thin layer detects: according to " Chinese Pharmacopoeia 2005 version annex VIB thin-layered chromatography test, draw each 4 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water=5: 3: 1: 1 for developping agent, launch, take out, dry, spray with 1% ferric trichloride ethanolic solution;
5. interpretation of result: the testing result of different production batch Baihuadingchuan Pill test sample; In test sample chromatogram, on the position corresponding to scutelloside reference substance chromatogram, the spot of aobvious same color, negative sample is noiseless; Show that test sample contains ingredients of Scutellaria;
(5) thin-layered chromatography differentiates semen armeniacae amarae: adopting thin-layered chromatography, take semen armeniacae amarae as control medicinal material, differentiates semen armeniacae amarae in Baihuadingchuan Pill prescription;
1. the preparation of need testing solution: get the need testing solution under above-mentioned root of large-flowered skullcap discriminating item;
2. the preparation of control medicinal material solution: get semen armeniacae amarae control medicinal material 1g, add methyl alcohol 15ml, adds hot reflux 30 minutes, lets cool, and filter, filtrate is medicinal material solution in contrast;
3. the preparation of negative sample solution: by prescription proportioning, get other flavour of a drug except semen armeniacae amarae, make pill according to the technique under [method for making] item in " Drug Standard of Ministry of Public Health of the Peoples Republic of China Traditional Chinese medicine historical preparation first " primary standard, then obtain negative sample solution by above-mentioned need testing solution preparation method;
4. thin layer detects: according to " Chinese Pharmacopoeia 2005 version annex VIB thin-layered chromatography test, draw each 4 ~ 6 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl formate-methyl alcohol-formic acid-water=12: the upper solution of 4: 0.8: 0.2: 2 is for developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde ethanol and 3% perchloric acid=1: 1 mixed solution, is heated to spot development clear;
5. interpretation of result: the testing result of different production batch Baihuadingchuan Pill test sample; In test sample chromatogram, on the position corresponding to semen armeniacae amarae control medicinal material chromatogram, the spot of aobvious same color, negative sample is noiseless; Show that test sample contains semen armeniacae amarae composition;
(6) Syrups by HPLC Chinese ephedra: adopting the Chinese ephedra in Syrups by HPLC prescription Baihuadingchuan Pill, take ephedrine hydrochloride as reference substance;
1. the setting of liquid phase chromatogram condition: with reference to " in Chinese Pharmacopoeia 2005 version one, " tongxuan lifei pills " content assaying method is formulated; Be filling agent with octadecylsilane chemically bonded silica; Mobile phase: second eyeball-0.1% phosphoric acid solution=30: 870; Determined wavelength is 210nm, column temperature: 40 DEG C; Flow velocity: 1ml/ minute; Number of theoretical plate calculates by ephedrine hydrochloride peak and is not less than 5000; Adopt above-mentioned chromatographic condition, analyze, result to ephedrine hydrochloride and pseudoephedrine hydrochloride, adopt above-mentioned chromatographic condition, both can reach baseline separation;
2. the preparation of standard solution: get ephedrine hydrochloride reference substance appropriate, accurately weighed, add methyl alcohol and make the solution of every 1ml containing 60 μ g, to obtain final product;
3. the preparation of need testing solution: get this product in right amount, shred, get about 2g, accurately weighed, add zeyssatite 2g, grind well, put in apparatus,Soxhlet's, add strong ammonia solution 3ml, with ethanol 10ml gradation washing mortar etc., be transferred in the lump and put in apparatus,Soxhlet's, then it is appropriate to add diethyl ether, heating is back to extracting liquid colourless, and extract decompression is steamed near dry, and residue adds methanol hydrochloride solution 1 → 1000 makes dissolving, be transferred in 10ml measuring bottle, and be diluted to scale, shake up, filter, get subsequent filtrate, to obtain final product;
This method is with reference to " in Chinese Pharmacopoeia 2005 version one, " tongxuan lifei pills " content assaying method is formulated; In need testing solution preparation, according to the architectural characteristic of ephedrine hydrochloride composition, adopt surname extraction mode, liquor ammoniae fortis alkalizes, and ether makes Extraction solvent, is using extracting liquid colourless as extraction terminal; Shift incomplete phenomenon in view of in the preparation of " tongxuan lifei pills " need testing solution, using the washing lotion of the ethanol of use as instruments such as cleaning mortars, be incorporated in apparatus,Soxhlet's; Separately contain the not volatile solvents such as a small amount of ethanol in view of in extract, in view of ephedrine is secondary amine constituents, the volatile feature of tool, adopts low-temperature reduced-pressure to steam to the nearly mode done, makes need testing solution preparation method be tending towards reasonable;
4. the preparation of negative sample solution: the ingredients removing Chinese ephedra by prescription, by [method for making] in " Drug Standard of Ministry of Public Health of the Peoples Republic of China Traditional Chinese medicine historical preparation first " primary standard obtained sample, again by above-mentioned need testing solution preparation method, obtained negative sample solution;
5. measure: accurate absorption reference substance solution, need testing solution, negative sample solution and each 10 μ l of use solvent respectively, injection liquid chromatography, measures, to obtain final product;
6. interpretation of result: can be determined in test sample containing ephedrine hydrochloride by retention time; With reference to " under Chinese Pharmacopoeia 2005 version Chinese ephedra item, content limit calculates, and the hydrochloric ephedrine of every g sample should be 0.29mg; Can calculate the content obtaining ephedrine hydrochloride in Baihuadingchuan Pill according to chromatogram, this content and state-promulgated pharmacopoeia compare, and can judge that whether the Chinese ephedra content of test sample is qualified, and then judge the quality of Baihuadingchuan Pill of different manufacturers, different batches; In this laboratory sample Baihuadingchuan Pill prescription, Chinese ephedra accounts for 6.7% of prescription total amount, adds refined honey 130g calculate in preparation by every 100g fecula, and every g sample is about containing Chinese ephedra fecula 29.13mg; In view of Baihuadingchuan Pill is starch, according to Chinese Pharmacopoeia Commission's requirement, starch calculates content limit by 80% rate of transform and formulates as every g contains Chinese ephedra with ephedrine hydrochloride, and its molecular formula is C
10h
15nO.HCl counts, and must not be less than 0.20mg; Calculate by every ball, limit is ordered as every ball contains Chinese ephedra with ephedrine hydrochloride, and its molecular formula is C
10h
15nO.HCl counts, and must not be less than 1.8mg;
Described Baihuadingchuan Pill by tussilago 44g, dried orange peel 88g, the tuber of dwarf lilyturf 88g, root of Chinese trichosanthes 88g, radix glehniae 44g, gypsum 44g, fruit of Chinese magnoliavine 44g, balloonflower root 88g, moutan bark 88g, peppermint 88g, asparagus fern 88g, semen armeniacae amarae 88g, root of purple-flowered peucedanum 88g, root of large-flowered skullcap 88g, lily 88g, Chinese ephedra 88g, aster 88g 17 taste Chinese medicine forms, its preparation method is by above 17 tastes, be ground into fine powder, sieve, mixing, every 100g powder adds refined honey 120 ~ 130g and makes large honeyed bolus and get final product.
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| CN105223292A (en) * | 2015-10-16 | 2016-01-06 | 山东明仁福瑞达制药股份有限公司 | A kind of detection method of Chinese medicine diffusing-freeing lung rectifying medicinal preparation |
| CN105929053A (en) * | 2016-04-20 | 2016-09-07 | 广西壮族自治区梧州食品药品检验所 | Method for determining ephedrine hydrochloride in lung ventilating and regulating pill by using ASE-UPLC |
| CN105866278A (en) * | 2016-04-20 | 2016-08-17 | 广西壮族自治区梧州食品药品检验所 | Method for determining ephedrine hydrochloride in lung-regulating pills by ultra-performance liquid chromatography |
| CN105929057A (en) * | 2016-04-22 | 2016-09-07 | 广西壮族自治区梧州食品药品检验所 | Method for determining ephedrine hydrochloride in lung ventilating and regulating pill |
| CN111398508A (en) * | 2020-04-10 | 2020-07-10 | 山东中大千方制药有限公司 | Method for identifying paeonol in sophora flower-scutellaria ointment |
| CN113791165B (en) * | 2021-09-13 | 2023-09-26 | 湖南新汇制药股份有限公司 | Quality detection method for stir-fried fructus viticis standard decoction |
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