CN1369704A - Method for testing quality of acanthopanax leaf - Google Patents
Method for testing quality of acanthopanax leaf Download PDFInfo
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- CN1369704A CN1369704A CN 01104005 CN01104005A CN1369704A CN 1369704 A CN1369704 A CN 1369704A CN 01104005 CN01104005 CN 01104005 CN 01104005 A CN01104005 A CN 01104005A CN 1369704 A CN1369704 A CN 1369704A
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Abstract
The present invention provides a detecting method for the quality of changgashan wilsonil leaf for medicinal use. The fingerprint atlas of total flavone and total saponin will be obtained through electric atomizing mass spectrum after wilsonii leaf having been processed with sampling process flow of alkohol extractino, concentration, filtration and grease removal and the kinds of total flavone and total saponin can be finalized according to its fingerprint atlas as well as the contents of total flavone and total saponin can be detected out by utilizing ultroviolet-visible spectrophotometer.
Description
The invention belongs to the quality determining method of acanthopanax.
Wilsonii is the Acanthopanax Araliaceae, is one of Changbaishan area special product Chinese crude drug, is used as medicine with its dry root and rhizome usually, and commodity are called Radix Acanthopanacis Senticosi.Wilsonii has long medicinal history.The quality standard of its root and rhizome, stem has been listed pharmacopeia version in 1996 in, and studies show that in recent years contains abundant flavones with extensive pharmacologically active and oside compound in the acanthopanax, can further develop.And leaf as medicinal material, had the protection medicine resource, eco-friendly characteristics.Because the quality standard of acanthopanax excludes pharmacopeia, sets up a kind of quality testing means accurately and reliably, be crucial for the development and use of acanthopanax.
The quality determining method that the purpose of this invention is to provide a kind of acanthopanax.The electrospray ionization mass spectrum that utilizes the acanthopanax crude extract utilizes UV-VIS spectrophotometry to determine the content of general flavone in the acanthopanax, total saponin as finger-print, has guaranteed the accuracy and the advance of quality inspection standard.
The present invention utilizes the soft ionization mass-spectrometric technique that the crude extract of acanthopanax is detected, and according to the number and the distribution of flavones and saponin in the electron spray finger-print of the acanthopanax crude extract that obtains, the quality of acanthopanax is carried out preliminary assessment.This finger-print can clearly reflect because the place of production, flavones that collecting season brought and saponin kind different.The present invention considers that the glucoside unit of contained saponin in the acanthopanax is based on oleanolic acid, this principle of chromogenic reaction can take place based on oleanolic acid and vanillic aldehyde-concentrated sulphuric acid, as standard items, measure the acanthopanax total saponin content with oleanolic acid by the content of measuring oleanolic acid in total saponin hydrolysate.And content of total flavone is measured the employing rutin as standard items, and aluminium nitrate and flavone compound form the colour developing principle of complex and measure.
The present invention selects the ethanol of 60%-90% as solvent, takes by weighing the acanthopanax 60-100g that pulverized in the 2000ml flask, adds 360ml-1000ml 60%-90% ethanol, by ultrasonic Extraction 2-3 time, and 20-40min/ time, or hot dipping 2-3 time, 1-3h/ time; Merge extracted twice liquid and be concentrated into about 60-100ml, closely colourless with petroleum ether extraction again, lower floor's evaporate to dryness is become solids, accurately take by weighing 50mg in the 50ml volumetric flask, be flavones content test sample a after adding the ethanol constant volume, saturated extracting n-butyl alcohol is 4 times behind the water constant volume, merges the n-butanol layer of 4 extractions respectively, evaporated under reduced pressure, residue moves in the 50ml volumetric flask with dissolve with methanol, uses methanol constant volume, shake up, as the sample b of total saponin content mensuration.
The electron spray finger-print of sample obtains as follows: the sample solution a that takes a morsel, after the methyl alcohol dilution, do the electrospray ionization mass spectrum analysis.The electrospray ionization mass spectrum experiment condition is as follows: electrospray ionization source, positive and negative ion ionization mode, spray voltage 3.5-5.5kV.The injection pump sample introduction flows.Sweep limit m/z50-2000.Utilize the negative ion electrospray ionization mass spectrum to confirm the kind of flavones, in the m/z50-700 scope, have m/z301, m/z447, m/z463, m/z609 plasma; Utilize the positive ion electrospray ionization mass spectrum to confirm the kind of saponin, in the m/z900-1500 scope, have m/z1065, m/z1081, m/z1097, m/z1108, m/z1123, m/z1211, m/z1227, m/z1243, m/z1253, m/z1269, m/z1285 plasma.The total saponin content method for measuring is as follows: the oleanolic acid that precision takes by weighing about 15mg places the 10ml volumetric flask, adds methanol constant volume; Vanillic aldehyde is made into 8% ethanolic solution; Sulfuric acid is made into 72% (V/V) solution.
Pipette oleanolic acid standard solution 0 μ l-100 μ l and 50 μ l sample solution b place six small test tubes respectively with the micro syringe precision, volatilize solvent, add 8% vanillic aldehyde ethanolic solution 0.5ml respectively, 72% (V/V) sulfuric acid 5ml, shake up the back in 60 ℃ of water bath with thermostatic control heating 10min, put then and cool off 15min in the ice-water bath, reactant is as solution to be measured.
At first the visible absorption of bioassay standard solution under the 530-545nm wavelength made standard working curve, records the content of total saponin in the sample then according to typical curve.
The determination of total flavonoids method is as follows: the rutin of the about 10mg of precision weighing, place the 10ml volumetric flask, add the ethanol constant volume, pipette rutin standard solution 0 μ l-50 μ l and 25 μ l sample solution a place the 25ml volumetric flask respectively with the micro syringe precision, add 5% sodium nitrite 1.0ml respectively, shake up, static 5min, add 4% sodium hydroxide solution 5ml again, add 70% ethanol to scale, place 15min, the at first absorption of bioassay standard solution under the 490-510nm wavelength, make standard working curve, record content of total flavone in the sample according to typical curve then.
The sample pretreatment process of this method is comparatively simple, and extraction efficiency is higher.The electrospray ionization mass spectrum that utilizes acanthopanax extract is as finger-print, can clearly find out the mass discrepancy of the acanthopanax that the different places of production, Various Seasonal are gathered by the kind of flavones, saponin, in conjunction with the assay result of ultraviolet-visible spectrophotometer, can estimate again the quality of acanthopanax to general flavone, total saponin in the acanthopanax extract.
Embodiment provided by the invention is as follows:
Embodiment 1
(1). specimen preparation
Take by weighing the acanthopanax 60g that pulverized in the 2000ml flask, add 360ml 60% ethanol, ultrasonic Extraction three times, each 20 minutes; Merge extracted twice liquid and also be concentrated into about 100ml, closely colourless with petroleum ether extraction again, lower floor's evaporate to dryness is become solids, accurately take by weighing 50mg in the 50ml volumetric flask, be flavones content test sample a after adding the ethanol constant volume.Saturated extracting n-butyl alcohol is 4 times behind the water constant volume, merges the n-butanol layer of 4 extractions respectively, evaporated under reduced pressure, and residue moves in the 50ml volumetric flask with dissolve with methanol, uses methanol constant volume, shakes up, as the sample b of total saponin content mensuration.
(2) the electron spray finger-print of sample
The sample solution a that takes a morsel, be diluted to finite concentration with methyl alcohol after, do the electrospray ionization mass spectrum analysis.The electrospray ionization mass spectrum experiment condition is as follows: electrospray ionization source, positive and negative ion ionization mode, spray voltage 4.5kV.The injection pump sample introduction flows.Sweep limit m/z50-2000.Utilize the negative ion electrospray ionization mass spectrum to confirm the kind of flavones, in the m/z50-700 scope, have m/z301, m/z447, m/z463, m/z609 ion; Utilize the positive ion electrospray ionization mass spectrum to confirm the kind of saponin, in the m/z900-1500 scope, have m/z1065, m/z1081, m/z1097, m/z1108, m/z1123, m/z1211, m/z1227, m/z1243, m/z1253, m/z1269, m/z1285 plasma.
(3) total saponin content method for measuring:
The oleanolic acid that precision takes by weighing about 15mg places the 10ml volumetric flask, adds methanol constant volume; Vanillic aldehyde is made into 8% ethanolic solution; Sulfuric acid is made into 72% (V/V) solution.
Pipette oleanolic acid standard solution 0 μ l-100 μ l and 50 μ l sample solution b place six small test tubes respectively with the micro syringe precision, volatilize solvent, add 8% vanillic aldehyde ethanolic solution 0.5ml respectively, 72% (V/V) sulfuric acid 5ml, shake up the back in 60 ℃ of water bath with thermostatic control heating 10min, put then and cool off 15min in the ice-water bath, reactant is as solution to be measured.
At first the visible absorption of bioassay standard solution under the 530nm wavelength made standard working curve, records the content of total saponin in the sample then according to typical curve.
(4) determination of total flavonoids:
The rutin of the about 10mg of precision weighing, place the 10ml volumetric flask, add the ethanol constant volume, pipette rutin standard solution 0 μ l-50 μ l and 25 μ l sample solution a place six 25ml volumetric flasks respectively with the micro syringe precision, add 5% sodium nitrite 1.0ml respectively, shake up, static 5min, add 4% sodium hydroxide solution 5ml again, add 70% ethanol to scale, place 15min, the at first absorption of bioassay standard solution under the 490nm wavelength, make standard working curve, record content of total flavone in the sample according to typical curve then.
Embodiment 2
(1). specimen preparation
Take by weighing the acanthopanax 80g that pulverized in the 2000mL flask, add 640ml 80% ethanol, ultrasonic Extraction secondary, each 30 minutes; The sample b that obtains flavones content test sample a and measure according to the sample preparation steps of embodiment 1 as total saponin content.
(2) the electron spray finger-print of sample
The sample solution a that takes a morsel, be diluted to finite concentration with methyl alcohol after, do the electrospray ionization mass spectrum analysis.The electrospray ionization mass spectrum experiment condition is as follows: electrospray ionization source, positive and negative ion ionization mode, spray voltage 4.5kV.The injection pump sample introduction flows.Sweep limit m/z50-2000.Confirm the kind of flavones and saponin according to the step (2) of embodiment 1.
(3) total saponin content method for measuring:
Utilize among the embodiment 1 the total saponin content method for measuring under the 537.5nm wavelength, standard solution and sample solution to be measured, determine the content of total saponin in the sample.
(4) determination of total flavonoids:
Utilize the method for determination of total flavonoids among the embodiment 1 under the 510nm wavelength, standard solution and sample solution to be measured, determine content of total flavone in the sample.
Embodiment 3:
(1). specimen preparation
Take by weighing the acanthopanax 100g that pulverized in the 2000mL flask, add 1000ml 90% ethanol, ultrasonic Extraction secondary, each 40 minutes; The sample b that obtains flavones content test sample a and measure according to the sample preparation steps of embodiment 1 as total saponin content.
(2) the electron spray finger-print of sample
The sample solution a that takes a morsel, be diluted to finite concentration with methyl alcohol after, do the electrospray ionization mass spectrum analysis.The electrospray ionization mass spectrum experiment condition is as follows: electrospray ionization source, positive and negative ion ionization mode, spray voltage 5.5kV.The injection pump sample introduction flows.Sweep limit m/z50-2000.Confirm the kind of flavones and saponin according to the step (2) of embodiment 1.
(3) total saponin content method for measuring:
Utilize among the embodiment 1 the total saponin content method for measuring under the 545nm wavelength, standard solution and sample solution to be measured, determine the content of total saponin in the sample.
(4) determination of total flavonoids:
Utilize the method for determination of total flavonoids among the embodiment 1 under the 500nm wavelength, standard solution and sample solution to be measured, determine content of total flavone in the sample.
Embodiment 4:
(1). specimen preparation
Take by weighing the acanthopanax 60g that pulverized in the 2000mL flask, add 360ml 60% ethanol, 60 ℃ of hot dippings are extracted each 2 hours three times; The sample b that obtains flavones content test sample a and measure according to the sample preparation steps of embodiment 1 as total saponin content.
(2) the electron spray finger-print of sample
The sample solution a that takes a morsel, be diluted to finite concentration with methyl alcohol after, do the electrospray ionization mass spectrum analysis.The electrospray ionization mass spectrum experiment condition is as follows: electrospray ionization source, positive and negative ion ionization mode, spray voltage 4.5kV.The injection pump sample introduction flows.Sweep limit m/z50-2000.Confirm the kind of flavones and saponin according to the step (2) of embodiment 1.
(3) total saponin content method for measuring:
Utilize among the embodiment 1 the total saponin content method for measuring under the 545nm wavelength, standard solution and sample solution to be measured, determine the content of total saponin in the sample.
(4) determination of total flavonoids:
Utilize the method for determination of total flavonoids among the embodiment 1 under the 510nm wavelength, standard solution and sample solution to be measured, determine content of total flavone in the sample.
Embodiment 5:
(1). specimen preparation
Take by weighing the acanthopanax 80g that pulverized in the 2000mL flask, add 640ml 80% ethanol, 60 ℃ of hot dippings are extracted each 1 hour three times; The sample b that obtains flavones content test sample a and measure according to the sample preparation steps of embodiment 1 as total saponin content.
(2) the electron spray finger-print of sample
The sample solution a that takes a morsel, be diluted to finite concentration with methyl alcohol after, do the electrospray ionization mass spectrum analysis.The electrospray ionization mass spectrum experiment condition is as follows: electrospray ionization source, positive and negative ion ionization mode, spray voltage 3.5kV.The injection pump sample introduction flows.Sweep limit m/z50-2000.Confirm the kind of flavones and saponin according to the step (2) of embodiment 1.
(3) total saponin content method for measuring:
Utilize among the embodiment 1 the total saponin content method for measuring under the 537.5nm wavelength, standard solution and sample solution to be measured, determine the content of total saponin in the sample.
(4) determination of total flavonoids:
Utilize the method for determination of total flavonoids among the embodiment 1 under the 500nm wavelength, standard solution and sample solution to be measured, determine content of total flavone in the sample.
Embodiment 6:
(1). specimen preparation
Take by weighing the acanthopanax 100g that pulverized in the 2000mL flask, add 1000ml 90% ethanol, secondaries, each 3 hours are extracted in 60 ℃ of hot dippings; The sample b that obtains flavones content test sample a and measure according to the sample preparation steps of embodiment 1 as total saponin content.
(2) the electron spray finger-print of sample
The sample solution a that takes a morsel, be diluted to finite concentration with methyl alcohol after, do the electrospray ionization mass spectrum analysis.The electrospray ionization mass spectrum experiment condition is as follows: electrospray ionization source, positive and negative ion ionization mode, spray voltage 5.5kV.The injection pump sample introduction flows.Sweep limit m/z50-2000.Confirm the kind of flavones and saponin according to the step (2) of embodiment 1.
(3) total saponin content method for measuring:
Utilize among the embodiment 1 the total saponin content method for measuring under the 530nm wavelength, standard solution and sample solution to be measured, determine the content of total saponin in the sample.
(4) determination of total flavonoids:
Utilize the method for determination of total flavonoids among the embodiment 1 under the 490nm wavelength, standard solution and sample solution to be measured, determine content of total flavone in the sample.
Claims (1)
1. the quality determining method of an acanthopanax, it is characterized in that selecting the ethanol of 60%-90% as solvent, take by weighing the acanthopanax 60-100g that pulverized in the 2000ml flask, add 360ml-1000ml 60%-90% ethanol, by ultrasonic Extraction 2-3 time, 20-40min/ time, or hot dipping 2-3 time, 1-3h/ time; Merge extracted twice liquid and also be concentrated into about 60-100ml, closely colourless with petroleum ether extraction again, lower floor's evaporate to dryness is become solids, accurately take by weighing 50mg in the 50ml volumetric flask, be flavones content test sample a after adding the ethanol constant volume; Saturated extracting n-butyl alcohol is 4 times behind the water constant volume, merges the n-butanol layer of 4 extractions respectively, evaporated under reduced pressure, and residue moves in the 50ml volumetric flask with dissolve with methanol, uses methanol constant volume, shakes up, as the sample b of total saponin content mensuration;
The electron spray finger-print of sample obtains as follows: the sample solution a that takes a morsel, after the methyl alcohol dilution, do the electrospray ionization mass spectrum analysis, the electrospray ionization mass spectrum experiment condition is as follows: electrospray ionization source, positive and negative ion ionization mode, spray voltage 3.5-5.5kV, the injection pump sample introduction flows; Sweep limit m/z50-2000 utilizes the negative ion electrospray ionization mass spectrum to confirm the kind of flavones, utilizes the positive ion electrospray ionization mass spectrum to confirm the kind of saponin;
The total saponin content method for measuring is as follows: the oleanolic acid that precision takes by weighing about 15mg places the 10ml volumetric flask, adds methanol constant volume; Vanillic aldehyde is made into 8% ethanolic solution; Sulfuric acid is made into 72% (V/V) solution;
Pipette oleanolic acid standard solution 0 μ l-100 μ l and 50 μ l sample solution b place six small test tubes respectively with the micro syringe precision, volatilize solvent, add 8% vanillic aldehyde ethanolic solution 0.5ml respectively, 72% (V/V) sulfuric acid 5ml, shake up the back in 60 ℃ of water bath with thermostatic control heating 10min, put then and cool off 15min in the ice-water bath, reactant is as solution to be measured;
At first the visible absorption of bioassay standard solution under the 530-545nm wavelength made standard working curve, records the content of total saponin in the sample then according to typical curve;
The determination of total flavonoids method is as follows: the rutin of the about 10mg of precision weighing, place the 10ml volumetric flask, add the ethanol constant volume, pipette rutin standard solution 0 μ l-50 μ l and 25 μ l sample solution a place the 25ml volumetric flask respectively with the micro syringe precision, add 5% sodium nitrite 1.0ml respectively, shake up, static 5min, add 4% sodium hydroxide solution 5ml again, add 70% ethanol to scale, place 15min, the at first absorption of bioassay standard solution under the 490-510nm wavelength, make standard working curve, record content of total flavone in the sample according to typical curve then.
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| CNB01104005XA CN1172178C (en) | 2001-02-16 | 2001-02-16 | Method for testing quality of acanthopanax leaf |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100412538C (en) * | 2005-11-10 | 2008-08-20 | 上海师范大学 | A test bar and its preparing process, and method for synchronous detecting rutin and vitamin C in medicine with the same testing bar |
| CN100465639C (en) * | 2006-06-07 | 2009-03-04 | 中国科学院长春应用化学研究所 | Inspection of manyprickle acanthopanax |
| CN101178389B (en) * | 2007-12-05 | 2010-12-15 | 广东省农业科学院农业生物技术研究所 | Method for identifying genuine-fake of black rice or produce therefrom by HPLC fingerprint |
| CN102512506A (en) * | 2012-01-01 | 2012-06-27 | 山东大学威海分校 | Compound acanthopanax root preparation capable of improving activity of superoxide dismutase |
| CN102727584A (en) * | 2012-06-29 | 2012-10-17 | 厦门牡丹香化实业有限公司 | Method for extracting flavonoids from camphor tree leaves |
| CN102899378A (en) * | 2012-10-18 | 2013-01-30 | 昆明理工大学 | Method for biotransformation of Panax notoginseng (Burk.) F. H. Chen medicinal material by using Monascus purpureus |
| CN106093249A (en) * | 2016-08-25 | 2016-11-09 | 南京林业大学 | A kind of method determining Carpinus betulus leaf collection period |
| CN109090310A (en) * | 2018-10-11 | 2018-12-28 | 佳木斯大学 | A kind of medicinal herb tea of the immunity that tonifies the kidney to relieve mental strain, improves and its preparation process |
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| CN101016287B (en) * | 2007-02-12 | 2010-07-28 | 西北农林科技大学 | Method of extracting flavone from cabbage leaf |
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- 2001-02-16 CN CNB01104005XA patent/CN1172178C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100412538C (en) * | 2005-11-10 | 2008-08-20 | 上海师范大学 | A test bar and its preparing process, and method for synchronous detecting rutin and vitamin C in medicine with the same testing bar |
| CN100465639C (en) * | 2006-06-07 | 2009-03-04 | 中国科学院长春应用化学研究所 | Inspection of manyprickle acanthopanax |
| CN101178389B (en) * | 2007-12-05 | 2010-12-15 | 广东省农业科学院农业生物技术研究所 | Method for identifying genuine-fake of black rice or produce therefrom by HPLC fingerprint |
| CN102512506A (en) * | 2012-01-01 | 2012-06-27 | 山东大学威海分校 | Compound acanthopanax root preparation capable of improving activity of superoxide dismutase |
| CN102727584A (en) * | 2012-06-29 | 2012-10-17 | 厦门牡丹香化实业有限公司 | Method for extracting flavonoids from camphor tree leaves |
| CN102899378A (en) * | 2012-10-18 | 2013-01-30 | 昆明理工大学 | Method for biotransformation of Panax notoginseng (Burk.) F. H. Chen medicinal material by using Monascus purpureus |
| CN106093249A (en) * | 2016-08-25 | 2016-11-09 | 南京林业大学 | A kind of method determining Carpinus betulus leaf collection period |
| CN109090310A (en) * | 2018-10-11 | 2018-12-28 | 佳木斯大学 | A kind of medicinal herb tea of the immunity that tonifies the kidney to relieve mental strain, improves and its preparation process |
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