CN101308123A - Liquid phase chromatography method for determining 8-O-acetyl Shanzhiside methylester content - Google Patents
Liquid phase chromatography method for determining 8-O-acetyl Shanzhiside methylester content Download PDFInfo
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- CN101308123A CN101308123A CNA2008101502777A CN200810150277A CN101308123A CN 101308123 A CN101308123 A CN 101308123A CN A2008101502777 A CNA2008101502777 A CN A2008101502777A CN 200810150277 A CN200810150277 A CN 200810150277A CN 101308123 A CN101308123 A CN 101308123A
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Abstract
The invention provides a method for measuring 8-O-acetyl geniposide methyl ester content in Lamiophlomis rotata Kudo by means of liquid phase chromatography, the method adopts an octadecylsilane chemically bonded silica as a filler, and acetonitrile-water as a mobile phase, and conducts the liquid phase chromatography analysis to the prepared sample solution under the chromatography conditions of detection wavelength of 230 to 240nm, flow rate of 0.5 to 2.0mL/min, and sample volume of 5 to 50-microlite, so as to measure the chromatographic peak area of the relevant position of a reference solution and calculate the corresponding content according to a standard curve. The measuring method of the invention is applied to Lamiophlomis rotata Kudo medicinal materials and extracts and preparations prepared by Lamiophlomis rotata Kudo medicinal materials.
Description
Technical field
The invention belongs to the field of Chinese medicines, relate to a kind of detection method of medicine, relate in particular to the method for 8-O-acetyl group Shanziside methyl ester content in a kind of liquid chromatography for measuring lamiophlomis rotata.
Background technology
Lamiophlomis rotata is traditional Tibetan medicine, and related preparations is by the pain easing and hemostasis of wide clinical application after various operations and the treatment of aspect such as department of stomatology, gynaecology, arthritis." Chinese pharmacopoeia requires to measure general flavone and content of luteolin in lamiophlomis rotata and the preparation thereof, and has set quality standard.It is that the iridoid glycoside constituents of representative has good hemostasis, analgesic activity that but a large amount of pharmacological evaluation show with 8-O-acetyl group Shanziside methyl ester, is the active substance basis of lamiophlomis rotata.Set up the content assaying method of 8-O-acetyl group Shanziside methyl ester in the common lamiophlomis root preparation, can ensure the quality of lamiophlomis rotata medicinal material and associated extraction thing thereof, preparation better.
Summary of the invention
The objective of the invention is for the method for 8-O-acetyl group Shanziside methyl ester content in a kind of liquid chromatography for measuring lamiophlomis rotata is provided.
The method of 8-O-acetyl group Shanziside methyl ester content in the liquid chromatography for measuring lamiophlomis rotata of the present invention; with the octadecylsilane chemically bonded silica is filling agent; acetonitrile-water is a moving phase; detecting wavelength 230～240nm; flow velocity 0.5～2.0mL/min under the chromatographic condition of sample size 5～50 μ l, carries out liquid-phase chromatographic analysis with the sample solution for preparing; measure the chromatographic peak area of reference substance solution relevant position, calculate corresponding content by typical curve.
Acetonitrile in the described moving phase: the volume ratio of water is 3: 100～40: 100 (the best is 15: 85).
The preparation of described reference substance solution: precision takes by weighing through the 8-O-of phosphorus pentoxide dried overnight acetyl group mountain Cape jasmine glycosides methyl esters reference substance, and water is made concentration between 0.1～100.0 μ gml
-1Gradient solution.
Assay method of the present invention is applicable to lamiophlomis rotata medicinal material and the extract and the preparation that are made by the lamiophlomis rotata medicinal material.
The preparation of described common lamiophlomis root preparation sample solution: common lamiophlomis root preparation is dissolved in the aqueous solution of any ratio of methyl alcohol or ethanol, the concentration that makes 8-O-acetyl group Shanziside methyl ester is between 0.1～100.0 μ gml
-1, promptly get sample solution.Wherein common lamiophlomis root preparation comprises tablet, capsule, granule, soft capsule, spreading agent, oral liquid, injection, film, aerosol, powder and external preparation.
The preparation of described lamiophlomis rotata medicinal material sample solution: with the lamiophlomis rotata medicinal material adopt that water is carried, alcohol extracting or ultrasonic Extraction, the gained extract is diluted to the concentration of 8-O-acetyl group Shanziside methyl ester between 0.1～100.0 μ gml
-1, promptly get sample solution.
The preparation of described common lamiophlomis root extract sample solution: common lamiophlomis root extract is dissolved in the aqueous solution of any ratio of methyl alcohol or ethanol, the concentration that is diluted to 8-O-acetyl group Shanziside methyl ester is between 0.1～100.0 μ gml
-1, promptly get sample solution.Common lamiophlomis root extract comprises the extract that various separation means obtain from the lamiophlomis rotata medicinal material, as lamiophlomis rotata water extract, lamiophlomis rotata total saponins, Radix Lamiophlomidis Rotatae total iridoid glycosides etc.
Below by concrete experiment the inventive method is further specified.
(1) instrument and reagent
High performance liquid chromatograph (U.S. Waters company), comprise 600 type binary gradient pumps, 996 type diode array UV-detector, BP210S electronic analytical balance (Sartorius company), SK7200H ultrasonic cleaner (Shanghai High Kudos Science Instrument Co., Ltd.).8-O-acetyl group mountain Cape jasmine glycosides methyl esters reference substance (laboratory self-control, MS, NMR determine its structure), purified water, acetonitrile is chromatographically pure (CaledonLaboratories LTD.Canada).5 kinds of market sale common lamiophlomis root preparations see Table 1.
The commercially available 5 kinds of common lamiophlomis root preparations of table 1
| Sample number into spectrum | The preparation title | Producer | The accurate word of authentication code traditional Chinese medicines | Lot number | Date of manufacture |
| 1 | The lamiophlomis rotata tablet | Baiyunshan Pharmaceutical General Factory | Z44020946 | 1070013 | 20070720 |
| 2 | Radix Lamiophlomidis Rotatae capsule | GanSu DuYiWei Biology Pharmacy Co., Ltd | Z10970053 | 0710025331 | 20071020 |
| 3 | Duyiwei soft capsule | Hainan Haishen Tongzhou Pharmaceutical Co., Ltd. | Z20050090 | 20080109 | 20080108 |
| 4 | Duyiwei soft capsule | Jiangsu Vanguard Pharmaceutical Co., Ltd. | Z20050221 | 0802291 | 20080229 |
| 5 | The lamiophlomis rotata granule | Chuanda Huaxi Pharmaceutical Industry Co., Ltd. Sichuan Prov. | Z20050308 | 070203 | 20070203 |
(2) chromatographic condition is selected
Symmetry C
18Chromatographic column (4.6mm * 150mm, 5 μ m, Waters); Wash-out moving phase is: acetonitrile-water (15: 85); Flow velocity 1.0mlmin
-120 ℃ of column temperatures; Sample size 20 μ l.
(3) selection of detection wavelength
Get 8-O-acetyl group mountain Cape jasmine glycosides methyl esters reference substance solution, in the interscan of 200～400nm scope, the result has absorption maximum at the 234nm place, so select 234nm as detecting wavelength.
(4) drafting of the investigation of linear dependence and typical curve
The accurate respectively 100 μ gml that draw
-1Control sample mother liquor 5.0,4.0,3.0,2.0,1.0ml adds to scale with water injection in the 25ml volumetric flask, concentration be respectively 20.0,16.0,12.0,8.0,4.0 μ gml
-1Gradient solution, accurate again draw solution 20.0 μ gml
-1Solution 2.5,1.5ml gets 2.0,1.2 μ gml with water injection dilution constant volume in the 25ml volumetric flask
-1Gradient solution integrates and obtains 1.2～20.0 μ gml
-17 gradient reference substance solution.Sample introduction 20 μ l measure chromatographic peak area respectively, are ordinate with the chromatographic peak area, and concentration is horizontal ordinate, and the drawing standard curve obtains linear equation and linearly dependent coefficient, the results are shown in Table 2.
Table 2 linear dependence is investigated the result
| Numbering | Concentration ug/ml | Peak area A |
| 1 | 1.2 | 27275 |
| 2 | 2 | 48555 |
| 3 | 4 | 95054 |
| 4 | 8 | 189406 |
| 5 | 12 | 278441 |
| 6 | 16 | 373401 |
| 7 | 20 | 472402 |
Investigate by the linear dependence of table 2 and to obtain linear equation and be:
Y=23459X+271.21; Linearly dependent coefficient r=0.9999.
Show that 8-O-acetyl group mountain Cape jasmine glycosides methyl esters is at 1.2～20.0 μ gml
-1Be the good linear relation with peak area in the concentration range.
(5) precision test
Precision is got 8.0 μ gml
-1Reference substance solution 20 μ l, respectively at first day, second day, the 3rd day respectively repeated sample introduction 5 times, and measured 8-O-acetyl group mountain Cape jasmine glycosides methyl esters peak integral area and retention time, and experimental result sees Table 3.
From the experimental result of table 3 as can be seen, in a few days, day to day precision, integral area in a few days RSD is respectively 0.08,0.13, with 0.52%, day to day precision RSD is 0.39%, and retention time in a few days RSD is respectively 0.18,1.44 and 0.31%, day to day precision RSD is 2.14%.
Table 3 Precision test result
(6) stability test
The same sample solution of accurate absorption is respectively 0,2,4,8,12,24, and 48h measures peak area integrated value (seeing Table 4), and meter RSD is 0.102%, shows that sample solution is basicly stable in 48 hours.
Table 4 stability test result
| Minute (h) | 0 | 2 | 4 | 8 | 12 | 24 | 48 |
| Integral area (A) | 185261 | 185567 | 185375 | 185211 | 185156 | 185076 | 185010 |
| The average integral area | 185237 | ||||||
| RSD(％) | 0.102 |
(7) reappearance test
According to the operation down of assay item, to measuring for 6 parts with a kind of lamiophlomis rotata sample, trying to achieve standard deviation RSD is 0.53%, the results are shown in Table 5.
Table 5 reproducible test results
(8) average recovery test
Get an amount of 9 parts of the sample of known sample content; 1-3 part adds reference substance 0.59mg; 4-6 part adds reference substance 0.984mg; 7-9 part adds reference substance 1.476mg; mixing prepares sample solution as stated above, measures chromatographic peak area as stated above; calculate the wherein content and the corresponding average recovery of 8-O-acetyl group mountain Cape jasmine glycosides methyl esters, the results are shown in Table 6.
The test of table 6 average recovery
(9) mensuration of lowest detectable limit
The accurate 8 μ gml that draw
-1Reference substance solution an amount of, be diluted to 8 with water for injection, 0.8ngml
-1Reference substance solution, respectively sample introduction 20 μ l measure chromatogram, should calculate by place's noise greater than 3 times with the chromatographic peak integral area, the detectability of 8-O-acetyl group mountain Cape jasmine glycosides methyl esters can reach 0.8ngml
-1, can satisfy the assay in the common lamiophlomis root preparation.
(10) assay in the sample
The accurate sample solution 20.0 μ l that draw; with above-mentioned chromatographic condition; inject high performance liquid chromatograph; measure chromatographic peak area with 8-O-acetyl group mountain Cape jasmine glycosides methyl esters standard items same position; calculate the content of 8-O-acetyl group mountain Cape jasmine glycosides methyl esters in the preparation according to typical curve; according to the preparation corresponding package, calculate 8-O-acetyl group mountain Cape jasmine glycosides methyl esters content in every (bag) simultaneously, the results are shown in Table 7.
Table 7 sample size is measured (n=2)
The result shows in the different preparations of lamiophlomis rotata all can detect 8-O-acetyl group mountain Cape jasmine glycosides methyl esters, but content differs greatly.
Embodiment
Embodiment one: Cape jasmine glycosides methyl esters Determination on content in 8-O-acetyl group mountain in the Radix Lamiophlomidis Rotatae capsule
Radix Lamiophlomidis Rotatae capsule is provided by GanSu DuYiWei Biology Pharmacy Co., Ltd, lot number: 0710025331.
Chromatographic condition and wavelength are selected: with octadecylsilane chemically bonded silica is filling agent; Acetonitrile-water (volume ratio is 15: 85) is a moving phase; Detect wavelength 234nm.
The preparation of reference substance solution: precision takes by weighing through the 8-O-of phosphorus pentoxide dried overnight acetyl group mountain Cape jasmine glycosides methyl esters reference substance an amount of, adds the injection water and makes the reference substance mother liquor that every 1ml contains 0.1mg.
The preparation of sample solution: precision takes by weighing Radix Lamiophlomidis Rotatae capsule content 1.0g in tool plug erlenmeyer flask, adds the methanol solution of 50ml 50%, claims to decide weight, in 70 ℃ of water-bath heating 30min, jolting constantly, it is fixed to claim after the cooling again, adds the weight that 50% methyl alcohol polishing loses.Filter, subsequent filtrate suitably dilutes, and promptly gets sample solution.
The preparation of typical curve: the accurate reference substance solution 5.0,4.0,3.0,2.0 of drawing, 1.0ml adds to scale with water for injection in the 25ml volumetric flask, get concentration and be respectively 20.0,16.0,12.0,8.0,4.0 μ gml
-1Gradient solution, accurate again draw solution 20.0 μ gml
-1Solution 2.5,1.5ml is in the 25ml volumetric flask, water for injection dilution constant volume gets 2.0,1.2 μ gml
-1Gradient solution integrates and obtains 1.2～20.0 μ gml
-1Between 7 gradient reference substance solution.Sample introduction 20 μ l measure chromatographic peak area respectively, are ordinate with the chromatographic peak area, and concentration is horizontal ordinate, the drawing standard curve.
Assay method: the accurate sample solution 20 μ l that draw; inject high performance liquid chromatograph; measure chromatographic peak area with the standard items relevant position; calculate according to typical curve that to contain 8-O-acetyl group Shanziside methyl ester in every 0.3g Radix Lamiophlomidis Rotatae capsule (being equivalent to crude drug 1g) be 3.11mg, promptly 8-O-acetyl group Shanziside methyl ester content is 1.033%.
Embodiment two: the mensuration of 8-O-acetyl group mountain Cape jasmine glycosides methyl esters in the lamiophlomis rotata tablet
The lamiophlomis rotata tablet is provided by Baiyunshan Pharmaceutical General Factory, lot number: 1070013.
Chromatographic condition and wavelength are selected: with octadecylsilane chemically bonded silica is filling agent; Acetonitrile-water (volume ratio 15: 85) is a moving phase; Detect wavelength 234nm.
The preparation of reference substance solution: precision takes by weighing through the 8-O-of phosphorus pentoxide dried overnight acetyl group mountain Cape jasmine glycosides methyl esters reference substance an amount of, adds the injection water and makes the reference substance mother liquor that every 1ml contains 0.1mg.
The preparation of sample solution: 20 in lamiophlomis rotata tablet, the place to go dressing grinds well, and precision takes by weighing 1.0g in tool plug erlenmeyer flask, add 50ml 50% methanol solution, claim to decide weight, in 70 ℃ of water-bath heating 30min, jolting constantly, it is fixed to claim after the cooling again, adds the weight that 50% methyl alcohol polishing loses.Filter, subsequent filtrate suitably dilutes, and promptly gets sample solution.
The preparation of typical curve: the accurate reference substance solution 5.0,4.0,3.0,2.0 of drawing, 1.0ml is in the 25ml volumetric flask, and water for injection adds to scale, gets concentration and is respectively 20.0,16.0,12.0,8.0,4.0 μ gml
-1Gradient solution, accurate again draw solution 20.0 μ gml
-1Solution 2.5,1.5ml is in the 25ml volumetric flask, water for injection dilution constant volume gets 2.0,1.2 μ gml
-1Gradient solution integrates and obtains 1.2-20.0 μ gml
-1Between 7 gradient reference substance solution.Sample introduction 20 μ l measure chromatographic peak area respectively, are ordinate with the chromatographic peak area, and concentration is horizontal ordinate, the drawing standard curve.
Assay method: the accurate sample solution 20 μ l that draw; inject high performance liquid chromatograph; measure chromatographic peak area with the standard items relevant position; calculate according to typical curve that to contain 8-0-acetyl group Shanziside methyl ester in every 0.28g lamiophlomis rotata tablet (being equivalent to crude drug 1g) be 3.0mg, promptly 8-0-acetyl group Shanziside methyl ester content is 1.073%.
Embodiment three: the mensuration of 8-O-acetyl group mountain Cape jasmine glycosides methyl esters in the lamiophlomis rotata medicinal material
The lamiophlomis rotata medicinal material picked up from the Maqu County, Gansu Province in 2007.8 months, was mainly its aerial part.
Chromatographic condition and wavelength are selected: with octadecylsilane chemically bonded silica is filling agent; Acetonitrile-water (volume ratio 15: 85) is a moving phase; Detect wavelength 234nm.
The preparation of reference substance solution: precision takes by weighing through the 8-O-of phosphorus pentoxide dried overnight acetyl group mountain Cape jasmine glycosides methyl esters reference substance an amount of, adds the injection water and makes the reference substance mother liquor that every 1ml contains 0.1mg.
The preparation of sample solution: the lamiophlomis rotata medicinal material, grind, cross 20 mesh sieves, precision takes by weighing 1.0g in the 250ml round-bottomed flask, adds the 50ml methanol solution, claims to decide weight, and in 75 ℃ of heating 30min that reflux, it is fixed to claim after the cooling again, adds the weight that the methyl alcohol polishing loses.Filter, subsequent filtrate suitably dilutes, and promptly gets sample solution.
The preparation of typical curve: the accurate reference substance solution 5.0,4.0,3.0,2.0 of drawing, 1.0ml is in the 25ml volumetric flask, and water for injection adds to scale, gets concentration and is respectively 20.0,16.0,12.0,8.0,4.0 μ gml
-1Gradient solution, accurate again draw solution 20.0 μ gml
-1Solution 2.5,1.5ml is in the 25ml volumetric flask, water for injection dilution constant volume gets 2.0,1.2 μ gml
-1Gradient solution integrates and obtains 1.2～20.0 μ gml
-1Between 7 gradient reference substance solution.Sample introduction 20 μ l measure chromatographic peak area respectively, are ordinate with the chromatographic peak area, and concentration is horizontal ordinate, the drawing standard curve.
Assay method: the accurate sample solution 20 μ l that draw; inject high performance liquid chromatograph; measure chromatographic peak area with the standard items relevant position; calculate according to typical curve that to contain 8-O-acetyl group Shanziside methyl ester in every 1g lamiophlomis rotata medicinal material be 8.0mg, promptly 8-O-acetyl group Shanziside methyl ester content is 0.80%.
Embodiment four: the mensuration of 8-O-acetyl group mountain Cape jasmine glycosides methyl esters in the only iridoid glycoside extract
The only iridoid glycoside extract is provided by the military region, Lanzhou Lanzhou Zong Yuan.
Chromatographic condition and wavelength are selected: with octadecylsilane chemically bonded silica is filling agent; Acetonitrile-water (volume ratio 15: 85) is a moving phase; Detect wavelength 234nm.
The preparation of reference substance solution: precision takes by weighing through the 8-O-of phosphorus pentoxide dried overnight acetyl group mountain Cape jasmine glycosides methyl esters reference substance an amount of, adds the injection water and makes the reference substance mother liquor that every 1ml contains 0.1mg.
The preparation of sample solution: precision takes by weighing only iridoid glycoside extract 0.1g in the 100ml volumetric flask, adds the injection water, constant volume, and suitably dilution promptly gets sample solution.
The preparation of typical curve: the accurate reference substance solution 5.0,4.0,3.0,2.0 of drawing, 1.0ml is in the 25ml volumetric flask, and water for injection adds to scale, gets concentration and is respectively 20.0,16.0,12.0,8.0,4.0 μ gml
-1Gradient solution, accurate again draw solution 20.0 μ gml
-1Solution 2.5,1.5ml is in the 25ml volumetric flask, water for injection dilution constant volume gets 2.0,1.2 μ gml
-1Gradient solution integrates and obtains 1.2～20.0 μ gml
-1Between 7 gradient reference substance solution.Sample introduction 20 μ l measure chromatographic peak area respectively, are ordinate with the chromatographic peak area, and concentration is horizontal ordinate, the drawing standard curve.
Assay method: the accurate sample solution 20 μ l that draw; inject high performance liquid chromatograph; measure chromatographic peak area with the standard items relevant position; calculate according to typical curve that to contain 8-O-acetyl group Shanziside methyl ester in every 1g only iridoid glycoside extract be 189.6mg, promptly 8-O-acetyl group Shanziside methyl ester content is 18.96%.
Claims (8)
1, the method for 8-O-acetyl group Shanziside methyl ester content in the liquid chromatography for measuring lamiophlomis rotata; it is characterized in that: be filling agent with the octadecylsilane chemically bonded silica; acetonitrile-water is a moving phase; detecting wavelength 230～240nm; flow velocity 0.5～2.0mL/min under the chromatographic condition of sample size 5～50 μ l, carries out liquid-phase chromatographic analysis with the sample solution for preparing; measure the chromatographic peak area of reference substance solution relevant position, calculate corresponding content by typical curve.
2, the method for 8-O-acetyl group Shanziside methyl ester content in the liquid chromatography for measuring lamiophlomis rotata according to claim 1 is characterized in that: described lamiophlomis rotata is lamiophlomis rotata medicinal material and the extract and the preparation that are made by the lamiophlomis rotata medicinal material.
3, the method for 8-O-acetyl group Shanziside methyl ester content in the liquid chromatography for measuring lamiophlomis rotata according to claim 1, it is characterized in that: acetonitrile in the described moving phase: the volume ratio of water is 3: 100～40: 100.
4, the method for 8-O-acetyl group Shanziside methyl ester content in the liquid chromatography for measuring lamiophlomis rotata according to claim 1; it is characterized in that: the preparation of described reference substance solution: precision takes by weighing through the 8-O-of phosphorus pentoxide dried overnight acetyl group mountain Cape jasmine glycosides methyl esters reference substance, and water is made concentration between 0.1～100.0 μ gml
-1Gradient solution.
5, the method for 8-O-acetyl group Shanziside methyl ester content in the liquid chromatography for measuring lamiophlomis rotata according to claim 1; it is characterized in that: the preparation of described common lamiophlomis root preparation sample solution: common lamiophlomis root preparation is dissolved in the aqueous solution of any ratio of methyl alcohol or ethanol, the concentration that makes 8-O-acetyl group Shanziside methyl ester is between 0.1～100.0 μ gml
-1, promptly get sample solution.
6, the method for 8-O-acetyl group Shanziside methyl ester content in the liquid chromatography for measuring lamiophlomis rotata according to claim 1; it is characterized in that: the preparation of described lamiophlomis rotata medicinal material sample solution: with the lamiophlomis rotata medicinal material adopt that water is carried, alcohol extracting or ultrasonic Extraction, the gained extract is diluted to the concentration of 8-O-acetyl group Shanziside methyl ester between 0.1～100.0 μ gml
-1, promptly get sample solution.
7, the method for 8-O-acetyl group Shanziside methyl ester content in the liquid chromatography for measuring lamiophlomis rotata according to claim 1; it is characterized in that: the preparation of described common lamiophlomis root extract sample solution: common lamiophlomis root extract is dissolved in the aqueous solution of any ratio of methyl alcohol or ethanol, the concentration that is diluted to 8-O-acetyl group Shanziside methyl ester is between 0.1～100.0 μ gml
-1, promptly get sample solution.
8, as the method for 8-O-acetyl group Shanziside methyl ester content in the liquid chromatography for measuring lamiophlomis rotata as described in the claim 5, it is characterized in that: described common lamiophlomis root preparation comprises tablet, capsule, granule, soft capsule, spreading agent, oral liquid, injection, film, aerosol, powder and external preparation.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101984983A (en) * | 2009-07-28 | 2011-03-16 | 甘肃独一味生物制药股份有限公司 | Lamiophlomis rotata extract, medicine composition containing same and quality control method thereof |
| CN101732405B (en) * | 2008-11-26 | 2013-02-06 | 甘肃独一味生物制药股份有限公司 | Common lamiophlomis extract, medicine composition containing same and quality control method |
| CN104127486A (en) * | 2014-07-22 | 2014-11-05 | 李茂星 | Application of total iridoid glycoside extract of Lamiophlomis rotata in preparation of constipation treatment medicines |
| CN104237441A (en) * | 2014-10-09 | 2014-12-24 | 成都中医药大学 | Method for simultaneous detection of iridoid glycoside, phenylethanoid glycoside, flavone and dicaffeoyl ingredients in lamiophlomis rotata |
-
2008
- 2008-07-01 CN CNA2008101502777A patent/CN101308123A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101732405B (en) * | 2008-11-26 | 2013-02-06 | 甘肃独一味生物制药股份有限公司 | Common lamiophlomis extract, medicine composition containing same and quality control method |
| CN101984983A (en) * | 2009-07-28 | 2011-03-16 | 甘肃独一味生物制药股份有限公司 | Lamiophlomis rotata extract, medicine composition containing same and quality control method thereof |
| CN101984983B (en) * | 2009-07-28 | 2013-03-13 | 甘肃独一味生物制药股份有限公司 | Detection method of Lamiophlomis rotata extract, medicine composition containing the extract |
| CN104127486A (en) * | 2014-07-22 | 2014-11-05 | 李茂星 | Application of total iridoid glycoside extract of Lamiophlomis rotata in preparation of constipation treatment medicines |
| CN104127486B (en) * | 2014-07-22 | 2017-07-18 | 李茂星 | Application of the Radix Lamiophlomidis Rotatae total iridoid glycosides extract in treatment constipation medicine is prepared |
| CN104237441A (en) * | 2014-10-09 | 2014-12-24 | 成都中医药大学 | Method for simultaneous detection of iridoid glycoside, phenylethanoid glycoside, flavone and dicaffeoyl ingredients in lamiophlomis rotata |
| CN104237441B (en) * | 2014-10-09 | 2015-07-22 | 成都中医药大学 | Method for simultaneous detection of iridoid glycoside, phenylethanoid glycoside, flavone and dicaffeoyl ingredients in lamiophlomis rotata |
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