CN103675135A - Content determination method of traditional Chinese medicine composition - Google Patents
Content determination method of traditional Chinese medicine composition Download PDFInfo
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Abstract
The invention belongs to the field of traditional Chinese medicines, and the invention discloses a content determination method of a traditional Chinese medicine composition. The method comprises (a) the preparation of a sample solution, (b) the preparation of a reference solution, (c) chromatographic conditions, to be more specific, a chromatographic column of C18 reversed phase chromatographic column, the column temperature of 30 DEG C, mobile phases of A acetonitrile and B trifluoroacetic acid solution, the gradient elution flow rate of 0.4ml / min, detection wavelengths of 230nm and 327nm, and (d) determination. The method is strong in specificity and simple in operation, and the quality of the traditional Chinese medicine composition can be effectively controlled.
Description
Technical field
The invention belongs to the field of Chinese medicines, be specifically related to a kind of content assaying method of Chinese medicine composition, the method adopts Ultra Performance Liquid Chromatography method to measure the content of chlorogenic acid, Paeoniflorin simultaneously.
Background technology
Traditional Chinese medicine is the history culture treasure-house of Chinese nation's brilliance, is the wisdom that clinical experience in several thousand accumulates.According to statistics, there are prescription more than 90,000 head, Chinese patent drug more than 5,000 kinds, 43 kinds of form of Chinese drug three the Fifteenth National Congress classes, 12,807 kinds of medicinal materials in China.Chinese medicine is the main method that the traditional Chinese medical science is cured the disease, and theory of traditional Chinese medical science is emphasized the overall utility of Chinese medicine, payes attention to the synergy of a plurality of chemical compositions in drug effect.But the standard that the quality control of Chinese medicine is mainly drafted with reference to < < Pharmacopoeia of People's Republic of China > > at present.The standard of most of Chinese medicine is only carried out quantitative test to single index components, fails to reflect the quality of preparation comprehensively.Therefore, new drug research is necessary to set up many indexs assay in quality standard, realizes the control to most component targets, and will the control of Chinese medicine preparation technical process directly be embodied in quality standard.
CN102688332A (Chinese Patent Application No.: 201110073726.4, date of publication: 2012.09.26) disclose a kind of Chinese medicine composition for the treatment of flu and preparation method thereof, present patent application is exactly the method for quality control research of carrying out for this Chinese medicine composition.
Summary of the invention
The content assaying method that the object of this invention is to provide two kinds of effective constituents of a kind of Chinese medicine composition.
This Chinese medicine composition is made by the bulk drug of following weight portion:
Cordate houttuynia 3～8, honeysuckle 3～8, the radix paeoniae rubrathe 1～5, peppermint 0.5～3, tarragon 1～5.
Aspect quality control, assay method provided by the invention can be measured the chlorogenic acid of this Chinese medicine composition, the content of two kinds of compositions of Paeoniflorin simultaneously, and method is simple, effective, feasible.
The object of the invention is to be achieved through the following technical solutions:
Chromatographic condition and system suitability test: chromatographic column is C18 reverse-phase chromatographic column; Mobile phase A is acetonitrile, Mobile phase B is trifluoroacetic acid solution, and gradient elution step is: 0～2 minute, and mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution is 5:95,2～15 minutes, mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution fades to 29:71 by 5:95; 15～20 minutes, mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution fades to 75:25 by 29:71; 20～25 minutes, mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution is 75:25; 25～50 ℃ of column temperatures; Detecting wavelength is 230nm and 327nm; Flow rate of mobile phase: 0.1～0.5ml/min, number of theoretical plate calculates and should be not less than 20000 by chlorogenic acid peak;
The preparation of reference substance solution: get chlorogenic acid and Paeoniflorin reference substance is appropriate, add methyl alcohol, obtain;
The preparation of need testing solution: get this Chinese medicinal composition preparation, accurately weighed, put in tool plug conical flask, add methyl alcohol, close plug, weighed weight, ultrasonic processing, lets cool, more weighed weight, supplies the weight of less loss with methyl alcohol, filters, and gets subsequent filtrate, obtains;
Assay method: precision is drawn reference substance solution and need testing solution 1～10 μ l respectively, injects Ultra Performance Liquid Chromatography instrument, measures, and by external standard method, calculates, and obtains.
The preferred version of said determination method is:
Chromatographic condition and system suitability test: chromatographic column is C18 reverse-phase chromatographic column; Mobile phase A is acetonitrile, Mobile phase B is 0.02% trifluoroacetic acid solution, and gradient elution step is: 0～2 minute, and mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution is 5:95,2～15 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution fades to 29:71 by 5:95; 15～20 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution fades to 75:25 by 29:71; 20～25 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution is 75:25; 30 ℃ of column temperatures; Detecting wavelength is 230nm and 327nm; Flow rate of mobile phase: 0.4ml/min, number of theoretical plate calculates and should be not less than 20000 by chlorogenic acid peak;
The preparation of reference substance solution: get chlorogenic acid and Paeoniflorin reference substance is appropriate, add 70% methyl alcohol and make every 1ml containing the solution of 0.1mg, 0.03mg, obtain;
The preparation of need testing solution: get this Chinese medicinal composition preparation, about 0.25g, accurately weighed, put in tool plug conical flask, precision adds 70% methyl alcohol 50ml, close plug, weighed weight, ultrasonic processing 30 minutes, lets cool, more weighed weight, with 70% methyl alcohol, supply the weight of less loss, 0.22 μ m miillpore filter filters, and gets subsequent filtrate, obtains;
Assay method: precision is drawn reference substance solution and each 2 μ l of need testing solution respectively, injects Ultra Performance Liquid Chromatography instrument, measures, and by external standard method calculating, obtains.
The weight ratio that adopts the inventive method to measure the described Chinese medicine composition Raw medicine of content is preferably: cordate houttuynia 5, honeysuckle 5, the radix paeoniae rubrathe 3, peppermint 1, tarragon 2.
Or cordate houttuynia 3, honeysuckle 3, the radix paeoniae rubrathe 1, peppermint 0.5, tarragon 1.
Or cordate houttuynia 7, honeysuckle 6, the radix paeoniae rubrathe 4, peppermint 2, tarragon 4.
Or cordate houttuynia 8, honeysuckle 8, the radix paeoniae rubrathe 5, peppermint 3, tarragon 5.
Or cordate houttuynia 4, honeysuckle 4, the radix paeoniae rubrathe 2, peppermint 1, tarragon 1.
Above-mentioned preferred Chinese medicine composition adopts this method to measure content all can obtain good precision and accuracy.
For content assaying method of the present invention is achieved, Chinese medicine composition of the present invention is made by the following step: extracting honeysuckle adds 50～70% ethanol, refluxing extraction 1～3 time, each 0.5～2 hour, extract filtered, merging filtrate, decompression recycling ethanol is also concentrated, drying under reduced pressure, pulverizes, and obtains extract powder I; Cordate houttuynia, tarragon, peppermint, add 5～10 times of water gagings, and steam distillation is extracted volatile oil, collects volatile oil, standby; Liquid is emitted, and another device is collected, and the dregs of a decoction and the radix paeoniae rubrathe add 5～15 times of water gagings, decoct, decocting liquid and above-mentioned liquid merge, and filter, filtrate decompression concentrates to obtain clear cream, is cooled to room temperature, adds ethanol and makes to reach 50～70% containing alcohol amount, standing, centrifugal, centrifugate decompression recycling ethanol is also concentrated, drying under reduced pressure, pulverize, obtain extract powder II; Volatile oil beta-cyclodextrin inclusion compound, inclusion compound dry, pulverize, standby; Extract powder I, II are mixed, add above-mentioned volatile oil clathrate compound, add the conventional pharmaceutic adjuvant in Chinese medicine preparation, adopt pharmaceutical methods conventional in pharmacy, preparations shaping, obtains.
In application of the present invention, described Chinese medicinal composition preparation formulation is tablet, buccal tablet, hard capsule, pill, granule, soft capsule, oral liquid, a kind of in spray for above-mentioned formulation can be realized, need add the acceptable auxiliary material of pharmacy, for example: filling agent when these formulations of preparation, disintegrant, lubricant, suspending agent, bonding agent, sweetener, flavouring, antiseptic etc., filling agent comprises: starch, pregelatinized starch, lactose, sweet mellow wine, chitin, microcrystalline cellulose, sucrose etc., disintegrant comprises: starch, pregelatinized starch, microcrystalline cellulose, sodium carboxymethyl starch, crospolyvinylpyrrolidone, low-substituted hydroxypropyl cellulose, cross-linked carboxymethyl cellulose is received etc., and lubricant comprises: dolomol, lauryl sodium sulfate, talcum powder, silicon dioxide etc., suspending agent comprises: polyvinylpyrrolidone, hydroxypropyl methylcellulose etc., sweetener comprises: saccharin sodium, aspartame, sucrose, honey element, enoxolone etc., flavouring comprises: sweetener and various essence, antiseptic comprises: parabens, benzoic acid, Sodium Benzoate, sorbic acid and its esters, benzalkonium bromide, acetic acid chloroethene is fixed, folium eucalypti wet goods.
For the effect of proved invention content assaying method, inventor has carried out a large amount of experiments and has carried out preferably, and final definite assay method has been carried out to the checking of science, and confirmatory experiment is as follows:
1 instrument and material
Agilent1290 liquid chromatograph, DAD UV-detector.
Acetonitrile is chromatographically pure (upper starfish can biochemical company limited), methyl alcohol is for analyzing pure (Nanjing Chemistry Reagent Co., Ltd.), trifluoroacetic acid is chromatographically pure (TEDIA COMPANY), water is self-control ultrapure water, chlorogenic acid reference substance (lot number: 110753-200413, National Institute for Food and Drugs Control), Paeoniflorin reference substance (lot number: 110736-201035, National Institute for Food and Drugs Control, purity: 96.5%), Chinese medicine composition tablet of the present invention is the (lot number: 120401 that Kangyuan Pharmaceutical Co., Ltd., Jiangsu Prov makes according to the preparation method of embodiment 1 preparation, 120701, 120702, 120703).
Determining of 2 chromatographic conditions
The preparation of test sample: get present composition tablet (lot number: 120401) 0.25g, accurately weighed, put in tool plug conical flask, precision adds 70% methyl alcohol 50ml, close plug, weighed weight, ultrasonic processing 30 minutes, let cool, more weighed weight, with 70% methyl alcohol, supply the weight of less loss, shake up, 0.22 μ m miillpore filter filters, and gets subsequent filtrate, obtains.
Chromatographic column is C18 reverse-phase chromatographic column, sample size 2 μ l.
2.1 elution programs are investigated
Mobile phase adopts gradient elution mode, using acetonitrile as mobile phase A, 0.02% trifluoroacetic acid solution is as Mobile phase B, 30 ℃ of column temperatures, flow velocity 0.4ml/min, it is 327nm that chlorogenic acid detects wavelength, it is 230nm that Paeoniflorin detects wavelength, elution program is in Table 1-1 and table 1-2, and chromatogram is shown in accompanying drawing 1～2.Result shows: elution program II separating effect is better.
Table 1-1 gradient elution program I
Table 1-2 gradient elution program II
2.2 flow velocitys are investigated
Elution program is as table 1-2,30 ℃ of column temperatures, and when investigating flow velocity and being respectively 0.3ml/min, 0.4ml/min, 0.5ml/min, the separating effect of composition to be measured, the results are shown in Table 2, and result shows: the velocity separation best results that adopts 0.4ml/min.
Table 2 different in flow rate is investigated result
2.3 column temperatures are investigated
Elution program is as table 1-2, and flow velocity is 0.4ml/min, the separating effect of composition to be measured when investigation column temperature is respectively 25 ℃, 30 ℃, 35 ℃, the results are shown in Table 3, show: different column temperature conditions, chromatographic peak all can obtain separation, but column temperature separated best results while being 30 ℃.
Table 3 column temperature is investigated
2.4 mobile phase concentration are investigated
Flow velocity 0.4ml/min, 30 ℃ of column temperatures, elution program is as table 1-2, and when investigation trifluoroacetic acid concentration distinguishes 0.01%, 0.02%, 0.05%, 0.1%, the separating effect of composition to be measured, the results are shown in Table 4.Result shows: while adopting 0.02% trifluoroacetic acid as Mobile phase B, chromatographic peak separating effect is best.
Table 4 trifluoroacetic acid concentration is investigated
2.5 wavelength are selected
The demonstration of DAD (190-600nm) scanning result, the maximum absorption wavelength of chlorogenic acid is 327.0nm, the maximum absorption wavelength of Paeoniflorin is 230.0nm, therefore adopt dual wavelength (chlorogenic acid 327nm, Paeoniflorin 230nm) to measure.
To sum up, determine that chromatographic condition is as follows:
Chromatographic column is C18 reverse-phase chromatographic column, mobile phase adopts gradient elution, take acetonitrile as mobile phase A, 0.02% trifluoroacetic acid is Mobile phase B, elution program is: 0～2 minute, mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution is 5:95,2～15 minutes, mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution fades to 29:71 by 5:95; 15～20 minutes, mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution fades to 75:25 by 29:71; 20～25 minutes, mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution is 75:25, column temperature is 30 ℃, flow velocity 0.4ml/min, detecting wavelength is 230nm and 327nm, sample size 2 μ l.
2.6 need testing solution extracting method tests
2.6.1 extracting mode is investigated
Get present composition tablet (lot number: 120401) 2 parts, every part of about 0.25g, accurately weighed, put in tool plug conical flask, precision adds methyl alcohol 50ml, weighed weight, ultrasonic processing and add hot reflux each 30 minutes respectively, more weighed weight, supplies the weight of less loss with 70% methyl alcohol, 0.22 μ m miillpore filter filters, and gets subsequent filtrate, as need testing solution, measurement result is in Table 5, result shows: two kinds of extracting mode differences are little, but ultrasonic extraction operation is more convenient, therefore select ultrasonic.
Table 5 extracting mode is selected
2.6.2 extracting solvent investigates
Get present composition tablet (lot number: 120401) 4 parts, every part of about 0.25g, accurately weighed, put in tool plug conical flask, precision adds methyl alcohol, 70% methyl alcohol, 50% methyl alcohol and ethanol 50ml, weighed weight respectively, ultrasonic processing 30 minutes, lets cool, more weighed weight, with coordinative solvent, supply the weight of less loss, 0.22 μ m miillpore filter filters, and gets subsequent filtrate, obtains, measurement result is in Table 6, and result shows: adopt ethanol lower for extracting 2 kinds of composition extraction ratios of solvent; Take 70% methyl alcohol as extracting solvent, and extraction ratio is higher.
Table 6 extracts solvent and selects
2.6.3 extraction time is investigated
Get present composition tablet (lot number: 120401) 3 parts, every part of about 0.25g, accurately weighed, to put in tool plug conical flask, precision adds 70% methyl alcohol 50ml, weighed weight, the ultrasonic processing time is respectively 15 minutes, 30 minutes, 45 minutes, lets cool, more weighed weight, with 70% methyl alcohol, supply the weight of less loss, shake up, 0.22 μ m miillpore filter filters, and gets subsequent filtrate, as need testing solution, carry out assay, measurement result is in Table 7, and result shows: under equal conditions, ultrasonic 30 minutes, extraction ratio was high.
Table 7 ultrasonic time is selected
2.6.4 extracting solvent load investigates
Get present composition tablet (lot number: 120401) 3 parts, every part of about 0.25g, accurately weighed, put in tool plug conical flask, precision adds 70% methyl alcohol 50ml, 75ml, 100ml, weighed weight respectively, ultrasonic processing 30 minutes, let cool, more weighed weight, with 70% methyl alcohol, supply the weight of less loss, shake up, 0.22 μ m miillpore filter filters, and gets subsequent filtrate, as need testing solution, carry out assay, the results are shown in Table 8, result shows: different solvents consumption is little on result impact, therefore select 50ml.
Table 8 extracts solvent volume and selects
Above result shows: take 70% methyl alcohol as extracting solvent, ultrasonic extraction 30 minutes, can make chlorogenic acid and Paeoniflorin in sample extract comparatively complete.
To sum up, the preparation method of need testing solution is as follows: get invention composite preparation, about 0.25g, accurately weighed, to put in tool plug conical flask, precision adds 70% methyl alcohol 50ml, close plug, weighed weight, ultrasonic processing 30 minutes, let cool, more weighed weight, with 70% methyl alcohol, supply the weight of less loss, shake up, 0.22 μ m miillpore filter filters, and gets subsequent filtrate, obtains.
3 methods and result
3.1 chromatographic conditions and system suitability
Chromatographic column is C18 reverse-phase chromatographic column; Mobile phase A is acetonitrile, Mobile phase B is 0.02% trifluoroacetic acid solution, gradient elution step is: 0～2 minute, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution is 5:95,2～15 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution fades to 29:71 by 5:95; 15～20 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution fades to 75:25 by 29:71; 20～25 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution is 75:25; 30 ℃ of column temperatures; Detecting wavelength is 230nm and 327nm; Flow rate of mobile phase: 0.4ml/min, number of theoretical plate calculates and should be not less than 20000 by chlorogenic acid peak;
The preparation of 3.2 reference substance solution
Get chlorogenic acid and Paeoniflorin reference substance is appropriate, add 70% methyl alcohol and make every 1ml containing the solution of 0.1mg, 0.03mg, obtain;
The preparation of 3.3 need testing solutions
Get present composition tablet (lot number: 120401), about 0.25g, accurately weighed, put in tool plug conical flask, precision adds 70% methyl alcohol 50ml, close plug, weighed weight, ultrasonic processing 30 minutes, lets cool, weighed weight again, the weight of supplying less loss with 70% methyl alcohol, shakes up, and 0.22 μ m miillpore filter filters, get subsequent filtrate, obtain;
3.4 linear relationships are investigated
Precision takes chlorogenic acid and Paeoniflorin reference substance is appropriate, adds methyl alcohol and makes hybrid standard stock solution (chlorogenic acid: 712.00 μ g/ml, Paeoniflorin: 209.21 μ g/ml).Stepwise dilution obtains serial reference substance solution, its Content of Chlorogenic Acid concentration is respectively: 356.0 μ g/ml, 213.60 μ g/ml, 142.40 μ g/ml, 106.80 μ g/ml, 53.40 μ g/ml, 26.70 μ g/ml, Paeoniflorin concentration is respectively: 104.60 μ g/ml, 62.76 μ g/ml, 41.84 μ g/ml, 31.38 μ g/ml, 15.69 μ g/ml, 7.845 μ g/ml, draw respectively above-mentioned solution 2 μ l, injection liquid chromatography, measure, the results are shown in Table 9, visible the method is good in trial stretch internal linear relation.
Table 9 typical curve and linear relationship experimental result
| Composition | Regression equation | Related coefficient | The range of linearity (μ g/ml) |
| Chlorogenic acid | Y＝15.164X-63.365 | 0.9997 | 26.70～356.00 |
| Paeoniflorin | Y＝6.828X-1.0032 | 1 | 7.845～104.60 |
3.5 stability test
Get same reference substance solution, need testing solution respectively at 0,2,4,8,12,18,24 hours sample introductions, the RSD of chlorogenic acid and Paeoniflorin reference substance solution is respectively 0.95%, 1.03%, and the RSD of need testing solution Content of Chlorogenic Acid, Paeoniflorin peak area is respectively 1.52%, 1.59%, show that reference substance solution and need testing solution are stable in 24 hours, measurement result is in Table 10-1,10-2.
Table 10-1 reference substance study on the stability result
Table 10-2 need testing solution Content of Chlorogenic Acid and Paeoniflorin study on the stability result
3.6 precision test
Get the chlorogenic acid (327nm) of variable concentrations and the need testing solution that Paeoniflorin (230nm) mixes contrast solution and preparation in continuous three days, continuous sample introduction is 6 times respectively, the results are shown in Table 11-1 and table 11-2, its peak area RSD (%) is all lower than 2%, result shows, instrument precision is good.
Table 11-1 precision is investigated
Table 11-2 test sample day to day precision is investigated
3.7 replica test
Get same lot number (120401) present composition tablet, repeat 6 sub-samplings, accurately weighed, by " 3.3 " described method, prepare need testing solution, sample introduction 2 μ l measure, calculate content, the average content of result preparation Content of Chlorogenic Acid is 2.37%, RSD=0.83%, and the average content of Paeoniflorin is 0.72%, RSD=1.25%, shows that this method repeatability is good.
3.8 recovery test
Accurately weighed present composition tablet (lot number: 120401), 6 parts, every part of about 0.125g, accurately weighed, put in 50ml measuring bottle, every part of precision adds chlorogenic acid reference substance solution (560.43 μ g/ml) 5ml and Paeoniflorin reference substance solution (130.76 μ g/ml) 5ml, precision adds 40ml70% methyl alcohol, weighed weight, ultrasonic processing 30 minutes, weighed weight again, with 70% methyl alcohol, supply the weight of less loss, shake up, 0.22 μ m miillpore filter filters, get subsequent filtrate, as need testing solution, carry out assay, measurement result is in Table 12-1, 12-2, result shows, the average recovery rate of chlorogenic acid and Paeoniflorin is respectively 100.05% and 96.57%, RSD is respectively 0.60% and 1.40%, test findings shows, the method recovery is good.
Table 12-1 chlorogenic acid application of sample reclaims result
Note: the recovery (%)=(amount of recording-sample size)/application of sample amount * 100%;
Sample Content of Chlorogenic Acid (mg)=sampling amount * 2.37% * 1000.
Table 12-2 Paeoniflorin application of sample reclaims result
Note: the recovery (%)=(amount of recording-sample size)/application of sample amount * 100%;
Paeoniflorin content in sample (mg)=sampling amount * 0.72% * 1000.
3.9 sample determination
Get three batches of (lot numbers: 120701,120702,120703) present composition tablet, by " 3.3 " described method, prepare need testing solution, precision is drawn reference substance solution and each 2 μ l of need testing solution respectively, inject Ultra Performance Liquid Chromatography instrument, record chromatographic peak area, external standard method is calculated content, and measurement result is in Table 13.
Table 13 preparation Content of Chlorogenic Acid and paeoniflorin content measurement result
Beneficial effect of the present invention:
Compound Chinese medicinal preparation composition kind is complicated, contains a plurality of effective constituent, adopts single wavelength to measure a plurality of compositions simultaneously, can lose the detection sensitivity that some measures composition.Multi-wavelength content assaying method can address this problem well.The present invention adopts Ultra Performance Liquid Chromatography fado wavelength to measure the content of 2 kinds of effective constituents simultaneously, and under this chromatographic condition, 2 kinds of effective constituents all can be completely separated.Through precision, repeatability, recovery test, prove, the content that the method can 2 kinds of effective constituents of Accurate Determining, method is easy, quick, accurate.Guaranteeing that measurement result accurately under prerequisite, can improve the sensitivity of detection greatly.Its accuracy, stability all meet production requirement, and energy effective control for product quality, guarantees curative effect of medication.
Accompanying drawing explanation
Fig. 1 elution program I chromatogram
Fig. 2 elution program II chromatogram
This Chinese medicine composition tablet of Fig. 3 Ultra Performance Liquid Chromatography figure
Embodiment
Following embodiment is for illustrating the content assaying method of Chinese medicine composition of the present invention, but it can not form any restriction to scope of the present invention.
Embodiment 1
For the ease of the enforcement of this Chinese medicine composition content assaying method, this Chinese medicine composition is prepared as to tablet
Prescription:
Cordate houttuynia 833g honeysuckle 833g radix paeoniae rubrathe 500g tarragon 333g peppermint 167g
Preparation method:
Extracting honeysuckle adds 12 times of amount 50% ethanol, refluxing extraction 2 times, and each 0.5 hour, extract filtered, merging filtrate, decompression recycling ethanol is also concentrated, and drying under reduced pressure, pulverizes, and obtains extract powder I; Cordate houttuynia, tarragon, peppermint, add 8 times of water gagings, and steam distillation is extracted volatile oil 5.0 hours, collects volatile oil, standby; Liquid is emitted, and another device is collected, and the dregs of a decoction and the radix paeoniae rubrathe add 10 times of water gagings, decoct 2 times, each 1.0 hours, decocting liquid and above-mentioned liquid merged, filter, filtrate decompression is concentrated, is cooled to room temperature, add ethanol and make to reach 70% containing alcohol amount, standing 12 hours, centrifugal, centrifugate decompression recycling ethanol is also concentrated, drying under reduced pressure, pulverizes, and obtains extract powder II; Volatile oil beta-cyclodextrin inclusion compound, inclusion compound low temperature drying, pulverizes, standby; By extract powder I, II, volatile oil clathrate compound, starch mix, wet granulation, dry, whole grain, enters microcrystalline cellulose and dolomol,, mix, compressing tablet, makes 1000, film coating, obtains.
Content assaying method:
Chromatographic condition and system suitability test chromatographic column are C18 reverse-phase chromatographic column; Mobile phase A is acetonitrile, Mobile phase B is 0.02% trifluoroacetic acid solution, gradient elution step is: 0～2 minute, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution is 5:95,2～15 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution fades to 29:71 by 5:95; 15～20 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution fades to 75:25 by 29:71; 20～25 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution is 75:25; 30 ℃ of column temperatures; Detecting wavelength is 230nm and 327nm.Number of theoretical plate calculates and should be not less than 20000 by chlorogenic acid peak.
Chlorogenic acid is got in the preparation of reference substance solution and Paeoniflorin reference substance is appropriate, adds 70% methyl alcohol and makes every 1ml containing the solution of 0.1mg, 0.03mg, obtains.
This Chinese medicinal composition preparation is got in the preparation of need testing solution, and about 0.25g is accurately weighed, put in tool plug conical flask, precision adds 70% methyl alcohol 50ml, close plug, weighed weight, ultrasonic processing 30 minutes, lets cool, more weighed weight, with 70% methyl alcohol, supply the weight of less loss, 0.22 μ m miillpore filter filters, and gets subsequent filtrate, obtains.
Determination method is accurate reference substance solution and each 2 μ l of need testing solution of drawing respectively, inject Ultra Performance Liquid Chromatography instrument, measure, and obtain.
Every of this product contains honeysuckle with chlorogenic acid (C
16h
18o
9) meter, must not be less than 13.4mg, with Paeoniflorin (C
23h
28o
11) meter, must not be less than 4.8mg.
For the ease of the enforcement of this Chinese medicine composition content assaying method, this Chinese medicine composition is prepared as to pill
Prescription:
Cordate houttuynia 18g honeysuckle 18g radix paeoniae rubrathe 6g tarragon 6g peppermint 3g
Preparation method:
Extracting honeysuckle adds 12 times of amount 50% ethanol, refluxing extraction 2 times, and each 0.5 hour, extract filtered, merging filtrate, decompression recycling ethanol is also concentrated, and drying under reduced pressure, pulverizes, and obtains extract powder I; Cordate houttuynia, tarragon, peppermint, add 8 times of water gagings, and steam distillation is extracted volatile oil 5 hours, collects volatile oil, standby; Liquid is emitted, and another device is collected, and the dregs of a decoction and the radix paeoniae rubrathe add 10 times of water gagings, decoct 2 times, each 1.0 hours, decocting liquid and above-mentioned liquid merged, filter, filtrate decompression is concentrated, is cooled to room temperature, add ethanol and make to reach 70% containing alcohol amount, standing 12 hours, centrifugal, centrifugate decompression recycling ethanol is also concentrated, drying under reduced pressure, pulverizes, and obtains extract powder II; Volatile oil beta-cyclodextrin inclusion compound, inclusion compound low temperature drying, pulverizes, standby; Extract powder I, II are mixed, add above-mentioned volatile oil inclusion complex, with the ratio melting mixing of PEG-4000 with 1:3, methyl-silicone oil is made cooling medium, and dripping becomes dripping pill 1000 balls, obtains.
Content assaying method:
Chromatographic condition and system suitability test chromatographic column are C18 reverse-phase chromatographic column; Mobile phase A is acetonitrile, Mobile phase B is 0.02% trifluoroacetic acid solution, gradient elution step is: 0～2 minute, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution is 5:95,2～15 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution fades to 29:71 by 5:95; 15～20 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution fades to 75:25 by 29:71; 20～25 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution is 75:25; 30 ℃ of column temperatures; Detecting wavelength is 230nm and 327nm.Number of theoretical plate calculates and should be not less than 20000 by chlorogenic acid peak.
Chlorogenic acid is got in the preparation of reference substance solution and Paeoniflorin reference substance is appropriate, adds 70% methyl alcohol and makes every 1ml containing the solution of 0.1mg, 0.03mg, obtains.
This Chinese medicinal composition preparation is got in the preparation of need testing solution, and about 0.25g is accurately weighed, put in tool plug conical flask, precision adds 70% methyl alcohol 50ml, close plug, weighed weight, ultrasonic processing 30 minutes, lets cool, more weighed weight, with 70% methyl alcohol, supply the weight of less loss, 0.22 μ m miillpore filter filters, and gets subsequent filtrate, obtains.
Determination method is accurate reference substance solution and each 2 μ l of need testing solution of drawing respectively, inject Ultra Performance Liquid Chromatography instrument, measure, and obtain.
The every ball of this product contains honeysuckle with chlorogenic acid (C
16h
18o
9) meter, must not be less than 0.29mg, with Paeoniflorin (C
23h
28o
11) meter, must not be less than 0.058mg.
Embodiment 3
For the ease of the enforcement of this Chinese medicine composition content assaying method, this Chinese medicine composition is prepared as to hard capsule
Prescription:
Cordate houttuynia 943g honeysuckle 808g radix paeoniae rubrathe 540g tarragon 540g peppermint 270g
Preparation method:
Extracting honeysuckle adds 12 times of amount 50% ethanol, refluxing extraction 2 times, and each 0.5 hour, extract filtered, merging filtrate, decompression recycling ethanol is also concentrated, and drying under reduced pressure, pulverizes, and obtains extract powder I; Cordate houttuynia, tarragon, peppermint, add 8 times of water gagings, and steam distillation is extracted volatile oil 5 hours, collects volatile oil, standby; Liquid is emitted, and another device is collected, and the dregs of a decoction and the radix paeoniae rubrathe add 10 times of water gagings, decoct 2 times, each 1.0 hours, decocting liquid and above-mentioned liquid merged, filter, filtrate decompression is concentrated, is cooled to room temperature, add ethanol and make to reach 70% containing alcohol amount, standing 12 hours, centrifugal, centrifugate decompression recycling ethanol is also concentrated, drying under reduced pressure, pulverizes, and obtains extract powder II; Volatile oil beta-cyclodextrin inclusion compound, inclusion compound low temperature drying, pulverizes, standby; Extract powder I, II are mixed, add above-mentioned volatile oil clathrate compound, whole grain, encapsulated, make 1000.
Content assaying method:
Chromatographic condition and system suitability test chromatographic column are C18 reverse-phase chromatographic column; Mobile phase A is acetonitrile, Mobile phase B is 0.02% trifluoroacetic acid solution, gradient elution step is: 0～2 minute, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution is 5:95,2～15 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution fades to 29:71 by 5:95; 15～20 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution fades to 75:25 by 29:71; 20～25 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution is 75:25; 30 ℃ of column temperatures; Detecting wavelength is 230nm and 327nm.Number of theoretical plate calculates and should be not less than 20000 by chlorogenic acid peak.
Chlorogenic acid is got in the preparation of reference substance solution and Paeoniflorin reference substance is appropriate, adds 70% methyl alcohol and makes every 1ml containing the solution of 0.1mg, 0.03mg, obtains.
This Chinese medicinal composition preparation is got in the preparation of need testing solution, and about 0.25g is accurately weighed, put in tool plug conical flask, precision adds 70% methyl alcohol 50ml, close plug, weighed weight, ultrasonic processing 30 minutes, lets cool, more weighed weight, with 70% methyl alcohol, supply the weight of less loss, 0.22 μ m miillpore filter filters, and gets subsequent filtrate, obtains.
Determination method is accurate reference substance solution and each 2 μ l of need testing solution of drawing respectively, inject Ultra Performance Liquid Chromatography instrument, measure, and obtain.
Every of this product contains honeysuckle with chlorogenic acid (C
16h
18o
9) meter, must not be less than 15.20mg, with Paeoniflorin (C
23h
28o
11) meter, must not be less than 5.18mg.
Embodiment 4
For the ease of the enforcement of this Chinese medicine composition content assaying method, this Chinese medicine composition is prepared as to soft capsule
Prescription:
Cordate houttuynia 720g honeysuckle 720g radix paeoniae rubrathe 450g tarragon 450g peppermint 270g
Preparation method:
Extracting honeysuckle adds 12 times of amount 50% ethanol, refluxing extraction 2 times, and each 0.5 hour, extract filtered, merging filtrate, decompression recycling ethanol is also concentrated, and drying under reduced pressure, pulverizes, and obtains extract powder I; Cordate houttuynia, tarragon, peppermint, add 8 times of water gagings, and steam distillation is extracted volatile oil 5 hours, collects volatile oil, standby; Liquid is emitted, and another device is collected, and the dregs of a decoction and the radix paeoniae rubrathe add 10 times of water gagings, decoct secondary, each 1.0 hours, decocting liquid and above-mentioned liquid merged, filter, filtrate decompression is concentrated, is cooled to room temperature, add ethanol and make to reach 70% containing alcohol amount, standing 12 hours, centrifugal, centrifugate decompression recycling ethanol is also concentrated, drying under reduced pressure, pulverizes, and obtains extract powder II; Volatile oil beta-cyclodextrin inclusion compound, inclusion compound low temperature drying, pulverizes, standby; Extract powder I, II are mixed, add above-mentioned volatile oil clathrate compound, add appropriate soybean oil and right amount of auxiliary materials, mix, sieve, be pressed into 1000 of soft capsules, obtain.
Content assaying method:
Chromatographic condition and system suitability test chromatographic column are C18 reverse-phase chromatographic column; Mobile phase A is acetonitrile, Mobile phase B is 0.02% trifluoroacetic acid solution, gradient elution step is: 0～2 minute, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution is 5:95,2～15 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution fades to 29:71 by 5:95; 15～20 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution fades to 75:25 by 29:71; 20～25 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution is 75:25; 30 ℃ of column temperatures; Detecting wavelength is 230nm and 327nm.Number of theoretical plate calculates and should be not less than 20000 by chlorogenic acid peak.
Chlorogenic acid is got in the preparation of reference substance solution and Paeoniflorin reference substance is appropriate, adds 70% methyl alcohol and makes every 1ml containing the solution of 0.1mg, 0.03mg, obtains.
This Chinese medicinal composition preparation is got in the preparation of need testing solution, and about 0.25g is accurately weighed, put in tool plug conical flask, precision adds 70% methyl alcohol 50ml, close plug, weighed weight, ultrasonic processing 30 minutes, lets cool, more weighed weight, with 70% methyl alcohol, supply the weight of less loss, 0.22 μ m miillpore filter filters, and gets subsequent filtrate, obtains.
Determination method is accurate reference substance solution and each 2 μ l of need testing solution of drawing respectively, inject Ultra Performance Liquid Chromatography instrument, measure, and obtain.
Every of this product contains honeysuckle with chlorogenic acid (C
16h
18o
9) meter, must not be less than 11.58mg, with Paeoniflorin (C
23h
28o
11) meter, must not be less than 4.32mg.
For the ease of the enforcement of this Chinese medicine composition content assaying method, this Chinese medicine composition is prepared as to granule
Prescription:
Cordate houttuynia 833g honeysuckle 833g radix paeoniae rubrathe 416g tarragon 208g peppermint 208g
Preparation method:
Extracting honeysuckle adds 12 times of amount 50% ethanol, refluxing extraction 2 times, and each 0.5 hour, extract filtered, merging filtrate, decompression recycling ethanol is also concentrated, and drying under reduced pressure, pulverizes, and obtains extract powder I; Cordate houttuynia, tarragon, peppermint, add 8 times of water gagings, and steam distillation is extracted volatile oil 5 hours, collects volatile oil, standby; Liquid is emitted, and another device is collected, and the dregs of a decoction and the radix paeoniae rubrathe add 10 times of water gagings, decoct secondary, each 1.0 hours, decocting liquid and above-mentioned liquid merged, filter, filtrate decompression is concentrated, is cooled to room temperature, add ethanol and make to reach 70% containing alcohol amount, standing 12 hours, centrifugal, centrifugate decompression recycling ethanol is also concentrated, drying under reduced pressure, pulverizes, and obtains extract powder II; Volatile oil beta-cyclodextrin inclusion compound, inclusion compound low temperature drying, pulverizes, standby; Extract powder I, II are mixed, add above-mentioned volatile oil clathrate compound, add appropriate sucrose, granulation, dry, make 1000g, obtain.
Content assaying method:
Chromatographic condition and system suitability test chromatographic column are C18 reverse-phase chromatographic column; Mobile phase A is acetonitrile, Mobile phase B is 0.02% trifluoroacetic acid solution, gradient elution step is: 0～2 minute, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution is 5:95,2～15 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution fades to 29:71 by 5:95; 15～20 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution fades to 75:25 by 29:71; 20～25 minutes, mobile phase acetonitrile: the volume ratio of 0.02% trifluoroacetic acid solution is 75:25; 30 ℃ of column temperatures; Detecting wavelength is 230nm and 327nm.Number of theoretical plate calculates and should be not less than 20000 by chlorogenic acid peak.
Chlorogenic acid is got in the preparation of reference substance solution and Paeoniflorin reference substance is appropriate, adds 70% methyl alcohol and makes every 1ml containing the solution of 0.1mg, 0.03mg, obtains.
This Chinese medicinal composition preparation is got in the preparation of need testing solution, and about 0.25g is accurately weighed, put in tool plug conical flask, precision adds 70% methyl alcohol 50ml, close plug, weighed weight, ultrasonic processing 30 minutes, lets cool, more weighed weight, with 70% methyl alcohol, supply the weight of less loss, 0.22 μ m miillpore filter filters, and gets subsequent filtrate, obtains.
Determination method is accurate reference substance solution and each 2 μ l of need testing solution of drawing respectively, inject Ultra Performance Liquid Chromatography instrument, measure, and obtain.
The every g of this product contains honeysuckle with chlorogenic acid (C
16h
18o
9) meter, must not be less than 13.4mg, with Paeoniflorin (C
23h
28o
11) meter, must not be less than 3.99mg.
Claims (10)
1. the content assaying method of a Chinese medicine composition Content of Chlorogenic Acid, Paeoniflorin, this Chinese medicine composition is made by the bulk drug of following weight portion: cordate houttuynia 3～8, honeysuckle 3～8, the radix paeoniae rubrathe 1～5, peppermint 0.5～3, tarragon 1～5, is characterized in that the method adopts Ultra Performance Liquid Chromatography method to measure, and comprises the following steps:
Chromatographic condition and system suitability test: chromatographic column is C18 reverse-phase chromatographic column; Mobile phase A is acetonitrile, Mobile phase B is trifluoroacetic acid solution, and gradient elution step is: 0～2 minute, and mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution is 5:95,2～15 minutes, mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution fades to 29:71 by 5:95; 15～20 minutes, mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution fades to 75:25 by 29:71; 20～25 minutes, mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution is 75:25; 25～50 ℃ of column temperatures; Detecting wavelength is 230nm and 327nm; Flow rate of mobile phase: 0.1～0.5ml/min, number of theoretical plate calculates and should be not less than 20000 by chlorogenic acid peak;
The preparation of reference substance solution: get chlorogenic acid and Paeoniflorin reference substance is appropriate, add methyl alcohol, obtain;
The preparation of need testing solution: get this Chinese medicinal composition preparation, accurately weighed, put in tool plug conical flask, add methyl alcohol, close plug, weighed weight, ultrasonic processing, lets cool, more weighed weight, supplies the weight of less loss with methyl alcohol, filters, and gets subsequent filtrate, obtains;
Assay method: precision is drawn reference substance solution and need testing solution 1～10 μ l respectively, injects Ultra Performance Liquid Chromatography instrument, measures, and by external standard method, calculates, and obtains.
2. content assaying method according to claim 1, is characterized in that, the methyl alcohol described in the method is that concentration is 50～90% methyl alcohol.
3. content assaying method according to claim 1, is characterized in that, mobile phase A is acetonitrile, and Mobile phase B is 0.02% trifluoroacetic acid solution.
4. content assaying method according to claim 1, is characterized in that, the method comprises the following steps:
Chromatographic condition and system suitability test: chromatographic column is C18 reverse-phase chromatographic column; Mobile phase A is acetonitrile, Mobile phase B is 0.02% trifluoroacetic acid solution, and gradient elution step is: 0～2 minute, and mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution is 5:95,2～15 minutes, mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution fades to 29:71 by 5:95; 15～20 minutes, mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution fades to 75:25 by 29:71; 20～25 minutes, mobile phase acetonitrile: the volume ratio of trifluoroacetic acid solution is 75:25; 30 ℃ of column temperatures; Detecting wavelength is 230nm and 327nm; Flow rate of mobile phase: 0.4ml/min, number of theoretical plate calculates and should be not less than 20000 by chlorogenic acid peak;
The preparation of reference substance solution: get chlorogenic acid and Paeoniflorin reference substance is appropriate, add 70% methyl alcohol and make every 1ml containing the solution of chlorogenic acid 0.1mg, Paeoniflorin 0.03mg, obtain;
The preparation of need testing solution: get this Chinese medicinal composition preparation, about 0.25g, accurately weighed, put in tool plug conical flask, precision adds 70% methyl alcohol 50ml, close plug, weighed weight, ultrasonic processing 30 minutes, lets cool, more weighed weight, with 70% methyl alcohol, supply the weight of less loss, 0.22 μ m miillpore filter filters, and gets subsequent filtrate, obtains;
Assay method: precision is drawn reference substance solution and each 2 μ l of need testing solution respectively, injects Ultra Performance Liquid Chromatography instrument, measures, and by external standard method calculating, obtains.
5. content assaying method according to claim 1, is characterized in that, this Chinese medicine composition is made by the bulk drug of following weight portion: cordate houttuynia 5, honeysuckle 5, the radix paeoniae rubrathe 3, peppermint 1, tarragon 2.
6. content assaying method according to claim 1, is characterized in that, this Chinese medicine composition is made by the bulk drug of following weight portion: cordate houttuynia 3, honeysuckle 3, the radix paeoniae rubrathe 1, peppermint 0.5, tarragon 1.
7. content assaying method according to claim 1, is characterized in that, this Chinese medicine composition is made by the bulk drug of following weight portion: cordate houttuynia 7, honeysuckle 6, the radix paeoniae rubrathe 4, peppermint 2, tarragon 4.
8. content assaying method according to claim 1, is characterized in that, this Chinese medicine composition is made by the bulk drug of following weight portion: cordate houttuynia 8, honeysuckle 8, the radix paeoniae rubrathe 5, peppermint 3, tarragon 5.
9. content assaying method according to claim 1, is characterized in that, this Chinese medicine composition is made by the bulk drug of following weight portion: cordate houttuynia 4, honeysuckle 4, the radix paeoniae rubrathe 2, peppermint 1, tarragon 1.
10. according to the content assaying method described in the arbitrary claim of claim 1-4, it is characterized in that, the preparation method of this Chinese medicine composition is: extracting honeysuckle adds 50～70% ethanol, refluxing extraction 1～3 time, each 0.5～2 hour, extract filters, merging filtrate, decompression recycling ethanol is also concentrated, drying under reduced pressure, pulverize, obtain extract powder I; Cordate houttuynia, tarragon, peppermint, add 5～10 times of water gagings, and steam distillation is extracted volatile oil, collects volatile oil, standby; Liquid is emitted, and another device is collected, and the dregs of a decoction and the radix paeoniae rubrathe add 5～15 times of water gagings, decoct, decocting liquid and above-mentioned liquid merge, and filter, filtrate decompression concentrates to obtain clear cream, is cooled to room temperature, adds ethanol and makes to reach 50～70% containing alcohol amount, standing, centrifugal, centrifugate decompression recycling ethanol is also concentrated, drying under reduced pressure, pulverize, obtain extract powder II; Volatile oil beta-cyclodextrin inclusion compound, inclusion compound dry, pulverize, standby; Extract powder I, II are mixed, add above-mentioned volatile oil clathrate compound, add the conventional pharmaceutic adjuvant in Chinese medicine preparation, adopt pharmaceutical methods conventional in pharmacy, preparations shaping, obtains.
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