CN101791366A - Method for testing quality of Discorea nipponica Makino in different places and medicinal materials of same genera - Google Patents
Method for testing quality of Discorea nipponica Makino in different places and medicinal materials of same genera Download PDFInfo
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Abstract
The invention provides a method for testing the quality of Discorea nipponica Makino and medicinal materials of dioscorea in different places. The method comprises the following steps: using medicinal material powder to be tested to prepare sample solutions, testing under a certain chromatographic conditions, and calculating the content of the indexes of each sample through external standard method, and the method is characterized in that dioscin and protodioscin are used as the content determination indexes. Dioscin and protodioscin are the main saponins components of dioscorea medicinal material, are active ingredients of Discorea nipponica Makino for reducing blood fat and are very important to control the quality of medicinal materials and preparations. The invention adopts RP-HPLC analysis method to test the contents of dioscin and protodioscin in Discorea nipponica Makino and medicinal materials of dioscorea in different places; and the method is sensitive, accurate and targeted and can be used to control the quality of medicinal materials, extracts and corresponding preparations.
Description
Technical field
The present invention relates to the field of Chinese crude drug quality testing, relate in particular to a kind of to different places of production Dioscorea nipponica Mak. Ningpo Yam Rhizome and belong to the method that medical material carries out quality testing together.
Background technology
Dioscorea nipponica Mak. Ningpo Yam Rhizome is used as medicine with rhizome, its effective ingredient is mainly steroid saponin, comprise different spirostane alcohol such as dioscin (dioscin) and cryptogenin (trillin) saponins, protodioscin (protodioscin) and former very thin saponin furostans such as (protogracillin) alcohol saponins.The total saponins hydrolysis produces diosgenin, and (diosgenin, average content Dio) are 0.93%～2.26%.Water soluble ingredient is separated right-acrinyl tartaric acid (Piscidicacid) has stronger antitussive effect.Still isolate in the rhizome a small amount of 2,5-D-spiral shell steroid-3, (25-D-Spirosta-3 5-diene), in addition, still contains compositions such as glucose, rhamnose, sterol, allantoin, resin, starch and protein to the 5-diene.
Dioscorea nipponica Mak. Ningpo Yam Rhizome has antiinflammatory, eliminates the phlegm, relievings asthma, increases coronary flow, blood fat reducing, improves cardiovascular function and pharmacologically actives such as antibiotic and antiviral, but decreased heart rate also, strengthen myocardial contraction, increase urine amount every day, improve coronary circulation, reduce arteriotony, be particularly useful for slight arteriosclerosis.Cure mainly diseases such as coronary heart disease, rheumatic fever, rheumatic arthritis, muscles and bones numbness, traumatic injury and bronchitis.Proof after deliberation in recent years, Dioscorea nipponica Mak. Ningpo Yam Rhizome also has contraception and effect such as anticancer, and medical value is very high, is one of primary raw material of domestic each big pharmaceutical factory developing new drug, special medicine and Chinese patent medicine, also is China's traditional export commodity.
" all detections under the discriminating of the Dioscorea nipponica Mak. Ningpo Yam Rhizome that Chinese pharmacopoeia is recorded and the assay item to diosgenin, belong to other four kinds of medical materials together and all do not record the assay item, and Dioscorea nipponica Mak. Ningpo Yam Rhizome and to belong to the saponin that contains in the medical material together of a great variety, complex structure, though the preparation assay is relatively more difficult with reference substance, but they all have identical basic framework and functional group, can be by the general character of skeleton or the characteristic of functional group, it is measured, the normal gravimetric method that adopts, colorimetry, polarimetry, coulometry and thin layer chromatography scanning, Tao Li etc. adopt the content of diosgenin in the gas chromatography determination Rhizoma Dioscoreae Zingiberensis, Zhao Jingchan etc. adopt the content of diosgenin in the positive high-performance liquid chromatogram determination Dioscorea nipponica Mak. Ningpo Yam Rhizome, all state employing reversed-phase high-performance liquid chromatography such as tiger, diode array detector is measured the content of diosgenin in the Dioscorea nipponica total saponins, and Tang Xiaoqing etc. adopt reversed-phase high-performance liquid chromatography, evaporative light scattering detector is measured the content of steroidal saponin in Radix Ophiopogonis.But these quantitative approach trivial operations, the method specificity is not strong, and accuracy of measurement is not high.
The Dioscorea nipponica Mak. Ningpo Yam Rhizome clinical practice is extensive, and DEVELOPMENT PROSPECT is preferably arranged.The effective ingredient of Dioscorea nipponica Mak. Ningpo Yam Rhizome is mainly steroid saponin, and steroidal saponin mainly is with the raw material of its aglycon as synthetic hormone class medicine at present, with the form of saponin as medicinal few.Therefore to reactive compound research of containing in the Dioscorea nipponica Mak. Ningpo Yam Rhizome important application prospects will be arranged.In addition, the quality standard of existing Dioscorea nipponica Mak. Ningpo Yam Rhizome medical material is more coarse, needs to set up more perfect method of quality control.
Summary of the invention
The invention provides a kind of to different places of production Dioscorea nipponica Mak. Ningpo Yam Rhizome and belong to the method that medical material carries out quality testing together, may further comprise the steps, medicinal powder to be measured is pressed the sample solution preparation manipulation, under certain chromatographic condition, measure, calculate each sample middle finger target content with external standard method, it is characterized in that choosing dioscin as the assay index.
Wherein, sample solution is that filtration prepared after medicinal powder was measured 60～70% ethanol ultrasonic extraction, 15～40min with 8～10 times.Preferred extraction process is 10 times of amount 65% ethanol ultrasonic extraction 30min, dioscin in the medical material can be extracted fully, and simple to operate, good reproducibility.
Sample can direct injected, sample introduction behind the n-butanol extraction, two step of ethyl acetate-n-butyl alcohol extraction back sample introduction after solvent extraction, preferred direct injected, and simple to operate, impurity is noiseless, good reproducibility.
Chromatographic condition is for being immobile phase with ODS, and volume ratio is that 55: 45 acetonitrile-water is a mobile phase, and the detection wavelength is 203nm, and flow velocity is 1.0mLmin
-1, column temperature is 35 ℃, sample size is 20 μ L.
Theoretical cam curve is calculated by dioscin and is not less than 3000; The separating degree of dioscin and adjacent peak is greater than 1.5; Symmetrical factor is pressed dioscin and is calculated all between 0.95～1.05.
By the dioscin curvilinear equation that settles the standard be: y=4.139 * 10
6X-7.023 * 10
4(r=0.9999).
The invention provides another kind of to different places of production Dioscorea nipponica Mak. Ningpo Yam Rhizome and belong to the method that medical material carries out quality testing together, may further comprise the steps, medicinal powder to be measured is pressed the sample solution preparation manipulation, under certain chromatographic condition, measure, calculate each sample middle finger target content with external standard method, it is characterized in that choosing protodioscin as the assay index.
Wherein, sample solution is after medicinal powder is measured 20～50% ethanol ultrasonic extraction, 15～40min with 8～10 times, to filter, and prepares after the two steps extraction of ethyl acetate-n-butyl alcohol.Preferred 10 times of amount 35% ethanol ultrasonic extraction 30min.When with 35% ethanol when extracting solvent, protodioscin extraction efficiency height, Interference Peaks is less, separating degree is better.Sample can direct injected, one step of n-butyl alcohol extraction back sample introduction, two step of ethyl acetate-n-butyl alcohol extraction back sample introduction after solvent extraction, two step of ethyl acetate-n-butyl alcohol extraction back sample introduction, and impurity is noiseless, good reproducibility.
Chromatographic condition is: be immobile phase with ODS, volume ratio is that 27: 73 acetonitrile-water is a mobile phase, and the detection wavelength is 203nm, and flow velocity is 1.0mLmin
-1, column temperature is 35 ℃, sample size is 20 μ L.
Theoretical cam curve is calculated by protodioscin and is not less than 1800; The separating degree of protodioscin and adjacent peak is greater than 1.5; Symmetrical factor is pressed protodioscin and is calculated all between 0.95～1.05.
By the protodioscin curvilinear equation that settles the standard be: y=4.462 * 10
6X-1.428 * 10
4(r=0.9999).
Contained steroidal saponin constituents is of a great variety in this genus medical material, and structural similarity is in end absorption in the ultra-violet (UV) band, and separating difficulty is bigger.But for the detectability of protodioscin and dioscin and precision, the repeatability of analytical method, UV-detector can reach pharmacopeia to methodological requirement, considers that UV-detector is comparatively commonly used, so select it as detector.For liquid phase chromatogram condition, once investigated the chromatographic column of different fillers, the methanol-water of different proportion, acetonitrile-water, acetonitrile-aqueous acetic acid, mobile phases such as acetonitrile-methanol-water, the result shows with Xterra
TMODS is an immobile phase, and acetonitrile-water is a mobile phase, and separating effect is best, and is highly sensitive.Detect by diode array detector, chromatographic peak purity height, analytical method has specificity.
Dioscin, protodioscin are the main saponin components in the Wild yam medical material, are the effective ingredient of Dioscorea nipponica Mak. Ningpo Yam Rhizome effect for reducing blood fat, therefore use dioscin, protodioscin as the assay index, and be very necessary to the quality of control medical material and preparation.The present invention adopts the RP-HPLC analytical method to measure the content of dioscin, protodioscin in the Dioscorea nipponica Mak. Ningpo Yam Rhizome of 27 collected separate sources and the Wild yam medical material, this method sensitivity, accurate, exclusive can be used for the quality control of medical material, extract and preparation thereof.
The specific embodiment
Introduce the present invention in detail below in conjunction with drawings and the specific embodiments; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also are considered as protection scope of the present invention.
Experiment material:
2695 type high performance liquid chromatograph U.S. Waters companies
2996 type diode array detector U.S. Waters companies
Empower work station U.S. Waters company
BP210S electronic balance Germany Sartorius company
RE-52A Rotary Evaporators Shanghai Yarong Biochemical Instrument Plant
The HH-2 numeral shows thermostat water bath Changzhou state China Instr Ltd.
Methanol (chromatographically pure) Concord, Tianjin Science and Technology Ltd.
Acetonitrile (chromatographically pure) Tian Jinsi friend biomedical technology company limited
Dehydrated alcohol (analytical pure) Guangzhou Chemical Reagent Factory
The redistilled water self-control
Protodioscin reference substance (purity 99.5%) self-control
Dioscin reference substance (purity 99.5%) self-control
Sample collection: this research has been collected different places of production Dioscorea nipponica Mak. Ningpo Yam Rhizome and has been belonged to totally 27 of medical material Dioscorea panthaica Prain et Burkill, Rhizoma Dioscoreae, Fen Rhizoma Dioscoreae Septemlobae, Mian Rhizoma Dioscoreae Septemlobae sample together.
Sample pretreatment: drying sample is pulverized, crossed 40 mesh sieves, put in the wide mouthed bottle airtight preservation.One, dioscin Determination on content
1, chromatographic condition
Chromatographic column: Xterra
TMODS (250mm * 4.6mm, 5 μ m), U.S. Waters company
Mobile phase: acetonitrile-water (55: 45, v/v)
Detect wavelength: 203nm
Flow velocity: 1.0mLmin
-1
Column temperature: 35 ℃
Sample size: 20 μ L
2, system suitability test
Get need testing solution, sample introduction analysis under above-mentioned chromatographic condition, theoretical cam curve is calculated by dioscin and is not less than 3000; The separating degree of dioscin and adjacent peak is greater than 1.5; Symmetrical factor is pressed dioscin and is calculated all between 0.95～1.05; Good reproducibility.
3, detecting wavelength selects
Get an amount of dioscin reference substance, dissolve wiring solution-forming with mobile phase, draw ultra-violet absorption spectrum, the maximum absorption wavelength of dioscin is 203nm, and this research selects 203nm for detecting wavelength.
4, sample solution preparation
The about 0.5g of material powder that gets it filled accurately claims surely, puts in the tool plug 100mL conical flask, adds 10 times and measures 65% ethanol, close plug, supersound process 30min.After extracting solution filtered, filtrate was put evaporate to dryness in the evaporating dish, and residue adds the mobile phase dissolving and quantitatively is transferred in the 25mL measuring bottle, is settled to scale with mobile phase, shakes up, and filters with 0.45 μ m microporous filter membrane, and it is standby to get subsequent filtrate.This is as sample solution.
5, standard curve is drawn
Get the about 100mg of dioscin reference substance, accurate claim surely, put in the 100mL measuring bottle, with the mobile phase dissolving and be settled to scale, make the reference substance solution that every 1mL contains dioscin 1.0mg, shake up.Precision is measured reference substance solution 1.0mL respectively, 2.0mL, and 3.0mL, 4.0mL, 6.0mL, 8.0mL place the 10mL measuring bottle, are diluted to scale with mobile phase, shake up, and get 0.1mgmL respectively
-1, 0.2mgmL
-1, 0.3mgmL
-11,0.4mgmL
-1, 0.6mgmL
-1, 0.8mgmL
-1The series reference substance solution.Accurate respectively each serial reference substance solution 20 μ L that draw inject high performance liquid chromatograph, and the record chromatogram is vertical coordinate (y) with the reference substance peak area, with reference substance solution concentration (mgmL
-1) be abscissa, the drawing standard curve, the result shows: dioscin is at 0.1～0.8mgmL
-1The scope internal linear is good, and gained regression curve equation is:
y＝4.139×10
6x-7.023×10
4(r＝0.9999)，
6, instrument precision test
The accurate dioscin reference substance solution 20 μ L that draw repeat sample introduction 6 times, inject high performance liquid chromatograph, and the record chromatogram is measured chromatographic peak area by above-mentioned chromatographic condition, calculates the relative standard deviation RSD=0.2% (n=6) of dioscin chromatographic peak area.
7, replica test
Take by weighing with 6 parts in a collection of Dioscorea nipponica Mak. Ningpo Yam Rhizome sample (Xinxiang, Henan), the accurate title, decide, by " preparation of a sample solution " method operation down, under above-mentioned chromatographic condition, the record chromatogram calculates content with external standard method, calculates the relative standard deviation RSD=0.4% (n=6) of dioscin content.
8, recovery test
Adopt the application of sample absorption method, take by weighing 9 parts in the Dioscorea nipponica Mak. Ningpo Yam Rhizome sample (Xinxiang, Henan) of known content, every part of about 0.25g accurately claims surely, accurately respectively adds basic, normal, high three kinds of concentration dioscin reference substance solution, by operating under " sample solution preparation ".Under above-mentioned chromatographic condition, measure the computational methods average recovery rate.The results are shown in Table 1.
The response rate of the dioscin of table 1, Dioscorea nipponica Mak. Ningpo Yam Rhizome sample
| Numbering | Raw material (mg) | Sample size (mg) | Addition (mg) | The response rate (%) | Average recovery rate (%) | ??RSD(％) |
| ??1 | ??8.22 | ??5.567 | ??2.805 | ??94.6 | ||
| ??2 | ??8.23 | ??5.489 | ??2.805 | ??97.8 | ||
| ??3 | ??8.27 | ??5.589 | ??2.805 | ??95.7 | ||
| ??4 | ??10.98 | ??5.580 | ??5.610 | ??96.2 | ||
| ??5 | ??11.14 | ??5.542 | ??5.610 | ??99.7 | ??97.9 | ??2.0 |
| ??6 | ??11.13 | ??5.489 | ??5.610 | ??100.0 | ||
| ??7 | ??13.86 | ??5.516 | ??8.41 | ??99.1 | ||
| ??8 | ??13.86 | ??5.562 | ??8.41 | ??98.6 | ||
| ??9 | ??13.90 | ??5.583 | ??8.41 | ??98.8 |
9, stability
Get same reference substance solution, at room temperature place, respectively at 0h, 2h, 4h, 6h, 8h, 10h, 12h, 24h, 48h and 72h sample introduction analysis under above-mentioned chromatographic condition, each 20 μ L, the record chromatographic peak area, calculate the RSD=1.7% of dioscin peak area, the result shows that the dioscin reference substance solution is stable in 72h.
10, sample determination
Get the dry medicinal powder of collected Dioscorea nipponica Mak. Ningpo Yam Rhizome and Wild yam thereof, operate down, under above-mentioned chromatographic condition, measure, calculate the content of dioscin in each sample, the results are shown in Table 3 with external standard method by " sample solution preparation ".
Two, protodioscin Determination on content
1, chromatographic condition
Chromatographic column: Xterra
TMODS (250mm * 4.6mm i.d., 5 μ m) U.S. Waters company
Mobile phase: acetonitrile-water (27: 73, v/v)
Detect wavelength: 203nm
Flow velocity: 1.0mLmin
-1
Column temperature: 35 ℃
Sample size: 20 μ L
2, system suitability test
Get need testing solution, sample introduction analysis under above-mentioned chromatographic condition, theoretical cam curve is calculated by protodioscin and is not less than 1800; The separating degree of protodioscin and adjacent peak is greater than 1.5; Symmetrical factor is pressed protodioscin and is calculated all between 0.95～1.05; Good reproducibility.
3, detecting wavelength selects
Get an amount of protodioscin reference substance, dissolve wiring solution-forming with mobile phase, draw ultra-violet absorption spectrum, the maximum absorption wavelength of protodioscin is 203nm, and this research selects 203nm for detecting wavelength.
4, sample solution preparation
The about 0.5g of material powder that gets it filled accurately claims surely, puts in the tool plug 100mL conical flask, adds 10 times and measures 35% ethanol, close plug, supersound process 30min.Extracting solution filters the back evaporate to dryness, and residue adds water 20mL dissolving, extracts 2 times with the ethyl acetate jolting, each 20mL, combining water layer extracts 3 times with water saturated n-butyl alcohol jolting, each 20mL, merge n-butyl alcohol liquid, decompression volatilizes solvent, and residue is dissolved in water and quantitatively is transferred in the 25mL measuring bottle, be settled to scale with mobile phase, shake up, filter with 0.45 μ m microporous filter membrane, it is standby to get subsequent filtrate.This is as sample solution.
5, standard curve is drawn
Get the about 100mg of protodioscin reference substance, accurate claim surely, put in the 100mL measuring bottle, with the mobile phase dissolving and be settled to scale, make the reference substance solution that every 1mL contains protodioscin 1.0mg, shake up.Precision is measured reference substance solution 0.2mL respectively, 0.5mL, and 1.0mL, 2.0mL, 3.0mL, 6.0mL place the 10mL measuring bottle, are diluted to scale with mobile phase, shake up, and get 0.02mgmL respectively
-1, 0.05mgmL
-1, 0.1mgmL
-1, 0.2mgmL
-1, 0.3mgmL
-1, 0.6mgmL
-1The series reference substance solution.Accurate respectively each serial reference substance solution 20 μ L that draw inject high performance liquid chromatograph, and the record chromatogram is vertical coordinate (y) with the reference substance peak area, with reference substance solution concentration (mgmL
-1) be abscissa, the drawing standard curve, the result shows: protodioscin is at 0.02～0.6mgmL
-1The scope internal linear is good.Gained regression curve equation is:
y＝4.462×10
6x-1.428×10
4(r＝0.9999)。
6, instrument precision test
The accurate protodioscin reference substance solution 20 μ L that draw, repeat sample introduction 6 times, inject high performance liquid chromatograph, the record chromatogram, measure chromatographic peak area by above-mentioned chromatographic condition, calculate the relative standard deviation RSD=0.2% (n=6) of protodioscin chromatographic peak area.
7, replica test
Take by weighing with 6 parts in a collection of Dioscorea nipponica Mak. Ningpo Yam Rhizome sample (Xinxiang, Henan), the accurate title, decide, by " sample solution preparation " method operation down, under above-mentioned chromatographic condition, the record chromatogram calculates content with external standard method, calculates the content relative standard deviation RSD=2.4% (n=6) of protodioscin.
8, recovery test
Adopt the application of sample absorption method, take by weighing 9 parts in the Dioscorea nipponica Mak. Ningpo Yam Rhizome sample (Xinxiang, Henan) of known content, every part of about 0.25g accurately claims surely, accurately respectively adds basic, normal, high three kinds of concentration protodioscin reference substance solution, by operating under " sample solution preparation ".Under above-mentioned chromatographic condition, measure the computational methods average recovery rate.The results are shown in Table 2.
The protodioscin response rate of table 2, Dioscorea nipponica Mak. Ningpo Yam Rhizome sample
9, stability
Get same reference substance solution, at room temperature place, respectively at 0,2,4,6,8,10,12,24,48 and 72h sample introduction analysis under above-mentioned chromatographic condition, each 20 μ L, the record chromatographic peak area, calculate the RSD=1.0% of protodioscin peak area, the result shows that the protodioscin reference substance solution is stable in 72h.
10, sample determination
Get collected Dioscorea nipponica Mak. Ningpo Yam Rhizome and Wild yam drying sample powder thereof, operate down, under above-mentioned chromatographic condition, measure, calculate the content of each sample Central Plains dioscin, the results are shown in Table 3 with external standard method by " sample solution preparation ".
Table 3, external standard method are calculated the content of dioscin and protodioscin in each sample
I: lot number is 121378-200401, ii: lot number is 121137-200402
" nd " meaning is not detect
The result shows, Dioscorea nipponica Mak. Ningpo Yam Rhizome is rich in protodioscin (content range is 11.24～27.05mgg in 5 kinds of Rhizoma Dioscoreae medical materials
-1), content takes second place in the Dioscorea panthaica Prain et Burkill, content is less in the Rhizoma Dioscoreae, detect in Rhizoma Dioscoreae Hypoglaucae, the Rhizoma Dioscoreae Septemlobae less than.In 5 kinds of Rhizoma Dioscoreae medical materials in the Dioscorea nipponica Mak. Ningpo Yam Rhizome dioscin content higher (content range is 17.31～28.59mgg
-1), content is less in the Dioscorea panthaica Prain et Burkill, and detect in the Rhizoma Dioscoreae, Rhizoma Dioscoreae Hypoglaucae, Rhizoma Dioscoreae Septemlobae less than.Reason may be relevant with the kind of the collecting season of medical material or medical material.
Claims (10)
1. one kind to different places of production Dioscorea nipponica Mak. Ningpo Yam Rhizome and belong to the method that medical material carries out quality testing together, may further comprise the steps, medicinal powder to be measured is pressed the sample solution preparation manipulation, under certain chromatographic condition, measure, calculate each sample middle finger target content with external standard method, it is characterized in that choosing dioscin as the assay index.
2. quality determining method as claimed in claim 1 is characterized in that, described sample solution is that filtration prepared after medicinal powder was measured 60～70% ethanol ultrasonic extraction, 15～40min with 8～10 times.
3. quality determining method as claimed in claim 1 is characterized in that, described chromatographic condition is, is immobile phase with ODS, and volume ratio is that the acetonitrile-water of 55:45 is a mobile phase, and the detection wavelength is 203nm.
4. quality determining method as claimed in claim 1 is characterized in that, described theoretical cam curve is calculated by dioscin and is not less than 3000.
5. quality determining method as claimed in claim 1 is characterized in that, by the dioscin curvilinear equation that settles the standard is: y=4.139 * 10
6X-7.023 * 10
4(r=0.9999).
6. one kind to different places of production Dioscorea nipponica Mak. Ningpo Yam Rhizome and belong to the method that medical material carries out quality testing together, may further comprise the steps, medicinal powder to be measured is pressed the sample solution preparation manipulation, under certain chromatographic condition, measure, calculate each sample middle finger target content with external standard method, it is characterized in that choosing protodioscin as the assay index.
7. quality determining method as claimed in claim 6 is characterized in that, described sample solution is that medicinal powder is measured 20～50% ethanol ultrasonic extraction, 15～40min after-filtration with 8～10 times, prepares after the two steps extraction of ethyl acetate-n-butyl alcohol.
8. quality determining method as claimed in claim 6 is characterized in that, described chromatographic condition is to be immobile phase with ODS, and volume ratio is that 27: 73 acetonitrile-water is a mobile phase, and the detection wavelength is 203nm.
9. quality determining method as claimed in claim 6 is characterized in that, described theoretical cam curve is calculated by protodioscin and is not less than 1800.
10. quality determining method as claimed in claim 6 is characterized in that, by the protodioscin curvilinear equation that settles the standard is: y=4.462 * 10
6X-1.428 * 10
4(r=0.9999).
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| CN104614482A (en) * | 2014-12-04 | 2015-05-13 | 天津世纪天龙药业有限公司 | Determination method for content of dioscin in Longjiatongluo capsule |
| CN106483224A (en) * | 2016-12-11 | 2017-03-08 | 江苏省中国科学院植物研究所 | The quick method measuring Smilax saponin B content in Rhizoma Dioscoreae Zingiberensiss |
| CN106501417A (en) * | 2016-12-11 | 2017-03-15 | 江苏省中国科学院植物研究所 | The quick method for determining protodioscin content in Rhizoma Dioscoreae Zingiberensiss |
| CN106706781A (en) * | 2016-12-11 | 2017-05-24 | 江苏省中国科学院植物研究所 | Method for rapid determination of content of dioscin in dioscorea zingiberensis |
| CN107356661A (en) * | 2017-07-26 | 2017-11-17 | 河南省科学院同位素研究所有限责任公司 | A kind of method for differentiating the Chinese yam place of production using Mineral Concentrations |
| CN113759036A (en) * | 2021-08-10 | 2021-12-07 | 北京康仁堂药业有限公司 | Method for measuring content of protodioscin in rhizoma dioscoreae septemlobae |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104614482A (en) * | 2014-12-04 | 2015-05-13 | 天津世纪天龙药业有限公司 | Determination method for content of dioscin in Longjiatongluo capsule |
| CN106483224A (en) * | 2016-12-11 | 2017-03-08 | 江苏省中国科学院植物研究所 | The quick method measuring Smilax saponin B content in Rhizoma Dioscoreae Zingiberensiss |
| CN106501417A (en) * | 2016-12-11 | 2017-03-15 | 江苏省中国科学院植物研究所 | The quick method for determining protodioscin content in Rhizoma Dioscoreae Zingiberensiss |
| CN106706781A (en) * | 2016-12-11 | 2017-05-24 | 江苏省中国科学院植物研究所 | Method for rapid determination of content of dioscin in dioscorea zingiberensis |
| CN107356661A (en) * | 2017-07-26 | 2017-11-17 | 河南省科学院同位素研究所有限责任公司 | A kind of method for differentiating the Chinese yam place of production using Mineral Concentrations |
| CN113759036A (en) * | 2021-08-10 | 2021-12-07 | 北京康仁堂药业有限公司 | Method for measuring content of protodioscin in rhizoma dioscoreae septemlobae |
| CN113759036B (en) * | 2021-08-10 | 2023-09-08 | 北京康仁堂药业有限公司 | Method for measuring content of protodioscin in rhizoma Dioscoreae Septemlobae |
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