CN103134890B - Detection method of giant knotweed rhizome and glossy privet gout capsules - Google Patents
Detection method of giant knotweed rhizome and glossy privet gout capsules Download PDFInfo
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- CN103134890B CN103134890B CN201310059961.5A CN201310059961A CN103134890B CN 103134890 B CN103134890 B CN 103134890B CN 201310059961 A CN201310059961 A CN 201310059961A CN 103134890 B CN103134890 B CN 103134890B
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- polydatin
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- 244000153955 Reynoutria sachalinensis Species 0.000 title claims abstract description 7
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- STKUCSFEBXPTAY-GSUVRYNNSA-N methyl (4s,5z,6s)-5-ethylidene-4-[2-oxo-2-[[(2r,3s,4s,5r,6r)-3,4,5-trihydroxy-6-[2-(4-hydroxyphenyl)ethoxy]oxan-2-yl]methoxy]ethyl]-6-[(2s,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy-4h-pyran-3-carboxylate Chemical compound O([C@@H]\1OC=C([C@H](C/1=C/C)CC(=O)OC[C@@H]1[C@H]([C@H](O)[C@@H](O)[C@H](OCCC=2C=CC(O)=CC=2)O1)O)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O STKUCSFEBXPTAY-GSUVRYNNSA-N 0.000 claims abstract description 30
- HSTZMXCBWJGKHG-UHFFFAOYSA-N (E)-piceid Natural products OC1C(O)C(O)C(CO)OC1OC1=CC(O)=CC(C=CC=2C=CC(O)=CC=2)=C1 HSTZMXCBWJGKHG-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229960003764 polydatin Drugs 0.000 claims abstract description 28
- HSTZMXCBWJGKHG-CUYWLFDKSA-N trans-piceid Polymers O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC(O)=CC(\C=C\C=2C=CC(O)=CC=2)=C1 HSTZMXCBWJGKHG-CUYWLFDKSA-N 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 229930182470 glycoside Natural products 0.000 claims description 30
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- 235000015266 Plantago major Nutrition 0.000 claims description 28
- LUKBXSAWLPMMSZ-OWOJBTEDSA-N Trans-resveratrol Polymers C1=CC(O)=CC=C1\C=C\C1=CC(O)=CC(O)=C1 LUKBXSAWLPMMSZ-OWOJBTEDSA-N 0.000 claims description 27
- 241000282376 Panthera tigris Species 0.000 claims description 22
- 239000013558 reference substance Substances 0.000 claims description 21
- 238000012360 testing method Methods 0.000 claims description 17
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 14
- 238000010828 elution Methods 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 7
- 239000012467 final product Substances 0.000 claims description 7
- 235000019253 formic acid Nutrition 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 241001499733 Plantago asiatica Species 0.000 claims description 4
- 235000013399 edible fruits Nutrition 0.000 claims description 4
- 238000004811 liquid chromatography Methods 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
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- 238000010812 external standard method Methods 0.000 claims description 2
- 238000011003 system suitability test Methods 0.000 claims description 2
- 238000004128 high performance liquid chromatography Methods 0.000 abstract description 5
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000011160 research Methods 0.000 abstract description 2
- KFEFLPDKISUVNR-QJEHNBJNSA-N Plantamajoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@H]1[C@H](OC(=O)\C=C\C=2C=C(O)C(O)=CC=2)[C@@H](CO)O[C@@H](OCCC=2C=C(O)C(O)=CC=2)[C@@H]1O KFEFLPDKISUVNR-QJEHNBJNSA-N 0.000 abstract 2
- DVXOEJHJQCHWHU-UHFFFAOYSA-N plantamajoside Natural products OCC1OC(OC2C(O)OC(CO)C(OC(=O)C=Cc3ccc(O)c(O)c3)C2O)C(O)C(OCCc4ccc(O)c(O)c4)C1O DVXOEJHJQCHWHU-UHFFFAOYSA-N 0.000 abstract 2
- KFEFLPDKISUVNR-NNBJPPDVSA-N purpureaside A Natural products OC[C@H]1O[C@@H](O[C@@H]2[C@@H](O)[C@H](OCCc3ccc(O)c(O)c3)O[C@H](CO)[C@H]2OC(=O)C=Cc2ccc(O)c(O)c2)[C@H](O)[C@@H](O)[C@@H]1O KFEFLPDKISUVNR-NNBJPPDVSA-N 0.000 abstract 2
- 239000012488 sample solution Substances 0.000 abstract 1
- 230000035945 sensitivity Effects 0.000 abstract 1
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- 239000000203 mixture Substances 0.000 description 8
- 238000011084 recovery Methods 0.000 description 7
- 239000003814 drug Substances 0.000 description 5
- 238000003556 assay Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- QNVSXXGDAPORNA-UHFFFAOYSA-N Resveratrol Natural products OC1=CC=CC(C=CC=2C=C(O)C(O)=CC=2)=C1 QNVSXXGDAPORNA-UHFFFAOYSA-N 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 238000010829 isocratic elution Methods 0.000 description 2
- 229940016667 resveratrol Drugs 0.000 description 2
- 235000021283 resveratrol Nutrition 0.000 description 2
- 206010018634 Gouty Arthritis Diseases 0.000 description 1
- 235000014676 Phragmites communis Nutrition 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 241000489523 Veratrum Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- -1 alcohol glycosides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019636 bitter flavor Nutrition 0.000 description 1
- 230000035619 diuresis Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007887 hard shell capsule Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
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- 238000013112 stability test Methods 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Medicinal Preparation (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a detection method of giant knotweed rhizome and glossy privet gout capsules. According to the invention, contents of polydatin, plantamajoside, specnuezhenide, and polydatin are determined by using a high performance liquid chromatography method. The method comprises the steps of sample solution preparation, control solution preparation, and determination. With the detection method provided by the invention, the contents of the four components of polydatin, plantamajoside, specnuezhenide, and polydatin can be simultaneously detected under a same chromatographic condition, such that operation steps of content determinations of the four components can be effectively simplified, determination time can be reduced, working efficiency can be improved, organic solvent application can be reduced, and effective control over the quality of giant knotweed rhizome and glossy privet gout capsules can be realized. The detection method has high sensitivity, good separation degree, and specificity. Accuracy, reproducibility, linear relationship, and stability of the method reach requirements of scientific researches and productions, such that the method can be popularized.
Description
Technical field
The invention belongs to medical technical field, be specifically related to the detection method of the loyal gout capsule of a kind of tiger.
Background technology
The loyal gout capsule of tiger is a kind of medicine for the treatment of urarthritis, and its prescription consists of giant knotweed, Asiatic plantain, the fruit of glossy privet, honeycomb.This medicine has clearing heat and promoting diuresis, and stagnation resolvation profit is turbid, and nourishing liver and kidney effect is mainly used in the primary acute gouty arthritis due to damp-heat accumulation.The preparation method of brave loyal gout capsule is taking ethanol as solvent, concentrated through extracting, and adds the dry rear filling of appropriate auxiliary material and forms.Specnuezhenide in polygonin in this medicine giant knotweed and polydatin, the fruit of glossy privet, the greater plantain glycosides in Asiatic plantain are the main survey indexs that contains wherein.The shortcomings such as at present, the quality standard of this existing medicine is to adopt different chromatographic conditions to measure respectively wherein a kind of content of composition, has complex operation, and detection time is long, testing cost height.In prior art, do not have about the bibliographical information of measuring the assay to polygonin, greater plantain glycosides, Specnuezhenide and four kinds of compositions of polydatin in the loyal gout capsule of tiger simultaneously.
Given this, be necessary the content assaying method of this medicine to study, to reduce minute, reduce costs, thereby the quality of the loyal gout capsule of tiger is effectively controlled.
Summary of the invention
The object of the present invention is to provide the detection method of the loyal gout capsule of a kind of tiger, the method can detect the content of polygonin, greater plantain glycosides, Specnuezhenide and four kinds of compositions of polydatin under same chromatographic condition simultaneously, effectively to control the quality of brave loyal gout capsule, ensure validity and the stability of product.
The present invention is achieved through the following technical solutions:
A detection method for the loyal gout capsule of tiger, the loyal gout capsule of described tiger is to be made up of giant knotweed, Asiatic plantain, the fruit of glossy privet, honeycomb,
With high effective liquid chromatography for measuring, specifically comprise the following steps:
(1) chromatographic condition and system suitability test: taking octadecylsilane chemically bonded silica as filling agent; Taking acetonitrile as mobile phase A, taking 0.1% formic acid solution as Mobile phase B, the regulation according to the form below is carried out gradient elution; Detection wavelength is 280nm, and flow velocity is 1.0ml/min, and theoretical cam curve is calculated and all should be not less than 3000 by polygonin peak, greater plantain glycosides peak, Specnuezhenide peak, polydatin peak;
| Time (minute) | Mobile phase A (%) | Mobile phase (B) |
| 0 | 16 | 84 |
| 25 | 30 | 70 |
| 30 | 30 | 70 |
(2) reference substance solution preparation: get respectively polygonin reference substance, greater plantain glycosides reference substance, Specnuezhenide reference substance, polydatin reference substance each appropriate, accurately weighed, add methyl alcohol and make every 1ml and be respectively containing polygonin, greater plantain glycosides, Specnuezhenide, polydatin the solution of 0.02-0.15mg, 0.05-0.15mg, 0.2-0.4mg, 0.1-0.3mg, to obtain final product;
(3) need testing solution preparation: get this product content 0.1g-0.3g, accurately weighed, it is the Diluted Alcohol 10-25ml of 50%-70% that precision adds volume ratio, weighed weight, ultrasonic processing 15-60 minute, is cooled to room temperature, more weighed weight, supply the weight of less loss with the Diluted Alcohol that volume ratio is 50%-70%, shake up, get supernatant, filter, get subsequent filtrate, to obtain final product;
(4) determination method: accurate reference substance solution and the each 10 μ l of need testing solution of drawing respectively, measure according to above-mentioned chromatographic condition, calculate and get final product by external standard method.
Preferably, in step (3), the volume ratio of described Diluted Alcohol is 50%.
The present invention compared with prior art, has following beneficial effect:
The detection method that the present invention formulates by the preparation of optimization chromatographic condition and test sample can detect the content of polygonin, greater plantain glycosides, Specnuezhenide and four kinds of compositions of polydatin under same chromatographic condition simultaneously, can effectively simplify the operation steps of the assay of these four kinds of compositions, reduce minute, improve work efficiency, reduce the use of organic solvent, be conducive to realize effective control of the quality to the loyal gout capsule of tiger.
Detection method of the present invention is highly sensitive, has good degree of separation, and detection method has specificity, and its accuracy, reappearance, linear relationship, stability all can reach the requirement of research and production, are suitable for applying.
Brief description of the drawings
Fig. 1 is that mobile phase is the HPLC collection of illustrative plates of acetonitrile-0.1% formic acid solution (16: 84) isocratic elution;
1 greater plantain glycosides 2 polygonin 3 Specnuezhenide 4 polydatins
Fig. 2 is the HPLC collection of illustrative plates of detection method of the present invention;
1 greater plantain glycosides 2 polygonin 3 Specnuezhenide 4 polydatins.
Embodiment
Further illustrate the present invention below by embodiment; following examples are the concrete embodiment of the present invention; but embodiments of the present invention are not subject to the restriction of following embodiment; other any do not deviate from change, the modification done under Spirit Essence of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
The phase Ⅲ clinical trial that embodiment detection method selects four meeting one power pharmaceutical Co. Ltds to produce is test sample with brave loyal gout capsule, and this product is hard shell capsules, and content is brown to tan powder; Mildly bitter flavor.
Polygonin is provided by Nat'l Pharmaceutical & Biological Products Control Institute, lot number 111575-200301.
Specnuezhenide is provided by Nat'l Pharmaceutical & Biological Products Control Institute, lot number 111926-201001(94.4%).
Greater plantain glycosides is provided by Nat'l Pharmaceutical & Biological Products Control Institute, lot number 111914-201102.
Polydatin is provided by Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 111535-200502.
embodiment 1the detection method of the loyal gout capsule of tiger
With high effective liquid chromatography for measuring, specifically comprise the following steps:
1) chromatographic condition: taking octadecylsilane chemically bonded silica as filling agent, taking acetonitrile as mobile phase A, taking 0.1% formic acid solution as Mobile phase B, the regulation according to the form below is carried out gradient elution; Detection wavelength is 280nm, and flow velocity is 1.0ml/min, and theoretical cam curve is calculated and all should be not less than 3000 by polygonin peak, greater plantain glycosides peak, Specnuezhenide peak, polydatin peak;
| Time (minute) | Mobile phase A (%) | Mobile phase (B) |
| 0 | 16 | 84 |
| 25 | 30 | 70 |
| 30 | 30 | 70 |
2) preparation of reference substance solution: get respectively polygonin reference substance, greater plantain glycosides reference substance, Specnuezhenide reference substance, polydatin reference substance each appropriate, accurately weighed, add methyl alcohol and make every 1ml and be respectively containing polygonin, greater plantain glycosides, Specnuezhenide, white black false hellebore the solution of 0.03mg, 0.08mg, 03mg, 0.2mg, obtain reference substance solution;
3) preparation of need testing solution: get this product content 0.15g, accurately weighed, it is 50% Diluted Alcohol 10ml that precision adds volume ratio, weighed weight, ultrasonic processing 30 minutes, is cooled to room temperature, more weighed weight, supply the weight of less loss with the Diluted Alcohol that volume ratio is 50%, shake up, get supernatant, filter, get subsequent filtrate, obtain need testing solution;
4) determination method: accurate reference substance solution and the each 10 μ l of need testing solution of drawing respectively, injection liquid chromatography, measures, and to obtain final product; Calculate according to the loyal gout capsule finished product of tiger, it is qualified that every gram of loyal gout capsule polygonin of tiger, greater plantain glycosides, Specnuezhenide, polydatin are no less than setting value.
Below the methodology of detection method of the present invention is investigated:
1, detect the selection of wavelength
The detection wavelength of " Chinese Pharmacopoeia " 2010 editions polygonins is 306nm, it is 330nm that greater plantain glycosides detects wavelength, it is 224nm that Specnuezhenide detects wavelength, and polydatin has absorption maximum at 300nm and 214nm place, content according to each composition in test sample and the response size in chromatographic condition thereof, selection 280nm is that the peak shape of the chromatographic peak of detection wavelength to polygonin, greater plantain glycosides, Specnuezhenide, polydatin is better, purity is high, therefore select 280nm as detection wavelength of the present invention.
2, the selection of mobile phase and elution requirement
Realize the assay of simultaneously measuring four kinds of compositions in brave loyal gout capsule under same chromatographic condition, the selection of mobile phase and elution requirement is gordian technique.
The selection of mobile phase of the present invention and elution requirement is adopted with the following method and is compared:
1) select acetonitrile-0.1% formic acid solution (16: 84) isocratic elution, its HPLC chromatogram as shown in Figure 1, Qi Zhonghu
Cane glycosides, greater plantain glycosides all went out peak about 20 minutes, are separated by 2 minutes, and Specnuezhenide went out peak at more than 30 minutes, and resveratrol reed alcohol glycosides just goes out peak about 70 minutes, and detection time is longer.
2) select mobile phase of the present invention and elution requirement: taking acetonitrile as mobile phase A, taking 0.1% formic acid solution as Mobile phase B, the regulation according to the form below is carried out gradient elution, its HPLC chromatogram as shown in Figure 2,
| Time (minute) | Mobile phase A (%) | Mobile phase (B) |
| 0 | 16 | 84 |
| 25 | 30 | 70 |
| 30 | 30 | 70 |
As seen from Figure 2, adopt above-mentioned gradient elution, polygonin, greater plantain glycosides, Specnuezhenide, four kinds of compositions of polydatin all went out peak in 30 minutes, and degree of separation is better, collection of illustrative plates baseline stability, therefore selecting acetonitrile is mobile phase A, carries out gradient elution taking 0.1% formic acid solution as Mobile phase B.
3, extract the selection of solvent
In pharmacopeia and document, adopt methyl alcohol or dilute methanol for extracting solvent to this Four content determination more, in order to reduce using and improving extraction ratio of organic solvent, the present invention adopts Diluted Alcohol to extract, and the concentration of ethanol is investigated, preferred volume ratio is that the Diluted Alcohol of 50%-70% extracts, the Diluted Alcohol that more preferably volume ratio is 50%.
4, methodology checking
(1) linear relationship is investigated accurate reference substance solution 2,4,6,8,10, the 12 μ l that draw, and injects respectively efficient
Liquid chromatograph, taking quality in sample size as horizontal ordinate X(ug), chromatographic peak area is ordinate Y, carries out linear regression, obtains regression equation: polygonin: Y=4E+06X – 224389, r=0.9999; Greater plantain glycosides: y=1982.3X-2.9E+5, r=0.9999; Specnuezhenide: y=92251X-24900, r=0.9999; Polydatin: y=48548X-7120, r=0.9998.
(2) precision is investigated the accurate reference substance solution 10 μ l that draw, repeat sample introduction 5 times, calculate average and the RSD value of each peak area, polygonin RSD is 0.70%, greater plantain glycosides RSD is 2.18%, Specnuezhenide RSD is 0.58%, polydatin RSD is 1.68%, and result shows that instrument precision is good.
(3) the loyal gout capsule of tiger that same lot number is got in stability test is prepared need testing solution, respectively 0,4,8,10, inject high performance liquid chromatograph and calculate each chromatographic peak area when 24h, the RSD of result polygonin chromatographic peak area is 2.04%, the RSD of greater plantain glycosides chromatographic peak area is 3.38%, the RSD of Specnuezhenide chromatographic peak area is 2.58, the RSD of polydatin chromatographic peak area is 2.21, and result shows that need testing solution is stable in 24 hours.
(4) the about 0.5g of the loyal gout capsule sample of tiger of same lot number is got in reappearance test, totally 6 parts, press need testing solution preparation method operation, inject high performance liquid chromatograph, measure in accordance with the law, result polygonin RSD is 1.58, and greater plantain glycosides RSD is 1.24, Specnuezhenide RSD is 1.19, polydatin RSD is 1.87, and result shows that this method reappearance is good.
(5) application of sample recovery test is got the loyal gout capsule 0.25g of tiger that content is known, totally 6 parts, 3 groups, point work, add respectively polygonin, greater plantain glycosides, Specnuezhenide, polydatin are appropriate, and by need testing solution, preparation method is prepared, measure calculate recovery rate and RSD in accordance with the law.Result shows, the average recovery rate of polygonin is 97.6%, RSD is 0.73%, the average recovery rate of greater plantain glycosides is 101.1, RSD is 3.04%, the average recovery rate of Specnuezhenide is that 98.9%, RSD is 1.54%, and the average recovery rate of polydatin is 99.2%, RSD is 2.07%, and the recovery meets the requirements.
the loyal gout capsule assay of tiger of embodiment 2 different lot numbers
Get the loyal gout capsule of tiger of different lot numbers, measure according to the content assaying method of embodiment 1, measure it and the results are shown in Table 1:
Result is surveyed in containing of 3 batches of each principal ingredients of the loyal gout capsule of tiger of table 1
| The loyal gout capsule of tiger | Determination of Polydatin (%) | Greater plantain glycosides content (%) | Specnuezhenide content (%) | Resveratrol content (%) |
| 120301 | 1.27 | 0.19 | 2.46 | 0.12% |
| 120302 | 1.08 | 0.22 | 1.85 | 0.15 |
| 120501 | 1.12 | 0.17 | 2.14 | 0.12 |
Claims (2)
1. a detection method for the loyal gout capsule of tiger, the loyal gout capsule of described tiger is by giant knotweed, Asiatic plantain, the fruit of glossy privet, honeycomb
Make, it is characterized in that, with high effective liquid chromatography for measuring, specifically comprise the following steps:
(1) chromatographic condition and system suitability test: taking octadecylsilane chemically bonded silica as filling agent; Taking acetonitrile as mobile phase A, taking 0.1% formic acid solution as Mobile phase B, the regulation according to the form below is carried out gradient elution; Detection wavelength is 280nm, and flow velocity is 1.0ml/min, and theoretical cam curve is calculated and all should be not less than 3000 by polygonin peak, greater plantain glycosides peak, Specnuezhenide peak, polydatin peak;
(2) reference substance solution preparation: get respectively polygonin reference substance, greater plantain glycosides reference substance, Specnuezhenide reference substance, polydatin reference substance each appropriate, accurately weighed, add methyl alcohol and make every 1ml and be respectively containing polygonin, greater plantain glycosides, Specnuezhenide, polydatin the solution of 0.02-0.15mg, 0.05-0.15mg, 0.2-0.4mg, 0.1-0.3mg, to obtain final product;
(3) need testing solution preparation: get this product content 0.1g-0.3g, accurately weighed, it is the Diluted Alcohol 10-25ml of 50%-70% that precision adds volume ratio, weighed weight, ultrasonic processing 15-60 minute, is cooled to room temperature, more weighed weight, supply the weight of less loss with the Diluted Alcohol that volume ratio is 50%-70%, shake up, get supernatant, filter, get subsequent filtrate, to obtain final product;
(4) determination method: accurate reference substance solution and the each 10 μ l of need testing solution of drawing respectively, measure according to above-mentioned chromatographic condition, calculate and get final product by external standard method.
2. the detection method of the loyal gout capsule of tiger according to claim 1, is characterized in that, in step (3), the volume ratio of described Diluted Alcohol is 50%.
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