CN101530463A - Quality detection method of Chinese herb gentian - Google Patents
Quality detection method of Chinese herb gentian Download PDFInfo
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- CN101530463A CN101530463A CN 200910066875 CN200910066875A CN101530463A CN 101530463 A CN101530463 A CN 101530463A CN 200910066875 CN200910066875 CN 200910066875 CN 200910066875 A CN200910066875 A CN 200910066875A CN 101530463 A CN101530463 A CN 101530463A
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Abstract
The invention provides a quality detection method of Chinese herb gentian. The method comprises the following steps: processing the gentian by sample pretreatment means of grinding, sifting, methanol ultrasound extracting, fixing volume and filtering, then obtaining finger-print of split iridoid glycoside component by electrospray ionization mass spectrometry, determining the species of the split iridoid glycoside component contained in the gentian according to the finger-print; measuring the content of the split iridoid glycoside compound by high performance liquid chromatography; synthesizing the finger-print and the content measurement data to evaluate the quality of the gentian. The quality detection method is accurate, quick, convenient and effective.
Description
Technical field
The invention belongs to technical field of Chinese medicines, be specifically related to quality detection method of Chinese herb gentian.
Technical background
The Chinese medicine Radix Gentianae is the dry root and rhizome of gentianaceae plant bar leaf Radix Gentianae (Gentiana manshuricaKitag.), Radix Gentianae (Gentianascabra Bge.), three flower Radix Gentianae (Gentiana triflora Pall.) or Gentiana rigescens Franch (Gentiana rigescens Franch.), first three is planted to practise and claims " Radix Gentianae ", and a kind of habit in back claims " Gentiana rigescens Franch ".Its discal patch leaf Radix Gentianae claims Northeastern Radix Gentianae again, and Radix Gentianae has another name called and is coarse Radix Gentianae.Radix Gentianae is cold in nature, and bitter in the mouth is returned the liver and gall warp, the tool heat clearing and damp drying, and eliminating pathogen in the liver gallbladder effect of fire belongs to heat clearing and dampness removing medicine.Be used for jaundice due to damp-heat, swelling of the vulva pudendal pruritus, leukorrhagia, eczema pruritus, conjunctival congestion deafness, diseases such as convulsion with spasms.Radix Gentianae is a conventional Chinese medicine, and the traditional Chinese medical science is got the property of its bitter cold, and eliminating pathogen in the liver gallbladder excess-fire is removed damp-heat in lower-JIAO.Discover that the root and rhizome of Radix Gentianae contains iridoid, secoiridoid and glycoside thereof, alkaloid, flavone, steroidal, coumarin, lactone, sugar and glycoside thereof, phenolic constituent, trace element, tannin, organic acid, volatilization wet goods volatile ingredient.Secoiridoid and glycoside thereof are the topmost drug activity composition of Chinese medicine Radix Gentianae, based on gentiopicrin, be hepatic cholagogic, be good for the stomach, the basic composition of pharmacological action such as antiinflammatory.Clinically, Radix Gentianae is the principal agent of prescriptions such as Decoction of Gentiana for Purging the Liver-fire, purging liver-fire ball, danggui longhui pills, danggui longhui wan, the merit of tool eliminating pathogen in the liver gallbladder excess-fire, clear damp-heat in lower-JIAO.Be used in recent years be good for the stomach, antitumor.Radix Gentianae Radix Gentianae in the world also is a crude drug, is recorded to be bitter stomachic.Chinese medicine Radix Gentianae kind is numerous on the market now, and chemical constituent between each kind and content are all variant, if chemical constituent and content can not reach prescription, will certainly influence the safety and the effectiveness of clinical practice.Safe and effective for guaranteeing that Chinese medicine uses, it is very necessary that Chinese crude drug is carried out quality testing accurately and reliably.(list of references: YangShaoyun (Yang Shaoyun), Wang Weiwei (Vera Wang), Li Zhiping (Li Zhiping) .ChineseTraditional Herb Drugs. (Chinese herbal medicine), 1981,12 (6): 7.)
Summary of the invention
The purpose of this invention is to provide a kind of quality detection method of Chinese herb gentian.This method utilizes the Electrospray Mass Spectrometry of Radix Gentianae crude extract as finger printing, utilizes high performance liquid chromatography to determine the content of Secoiridoid Glycosides chemical compound in the Radix Gentianae, has guaranteed the advance of the accuracy and the quality inspection standard of quality determining method.
It is as follows to implement technical scheme of the present invention:
The Chinese medicine Radix Gentianae was pulverized the 60-80 mesh sieve, take by weighing the Radix Gentianae 50-200mg that has pulverized and put in the 50ml conical flask, the methanol that with the concentration of volume percent is 50%-100% adds methanol 5-20ml as solvent, supersound extraction 1-3 time, 20-40min/ time, 20-50 ℃ of supersound extraction temperature filtered, merge said extracted liquid and be concentrated into 1-2ml, methanol constant volume shakes up to 10ml, is for test agent solution;
The electron spray finger printing of sample obtains as follows: get 50-100 μ L for test agent solution, after 10 times of methanol dilutions, do the Electrospray Mass Spectrometry analysis; The Electrospray Mass Spectrometry experiment condition is as follows: the electron spray ionisation source, and spray voltage 3.5-5.5kV, capillary temperature 180-220 ℃, injection pump sample introduction flow velocity 2-8 μ l/min flows; Sweep limits mass-to-charge ratio (m/z) 50-2000 utilizes the cation Electrospray Mass Spectrometry to confirm the kind of secoiridoid glycoside, under the cation condition, in m/z 100-1000 scope, have m/z 379, m/z 381, and m/z 395, m/z 735, and m/z 805, m/z 821 ions;
The high-efficient liquid phase chromatogram technology condition is as follows: C18 chromatographic column condition is 150mm * 4.6mm, 5 μ m, column temperature 20-35 ℃; Mobile phase is the first alcohol and water, methanol and water volume ratio 80:20-30:70, elution time 30-60min; UV-detector detects wavelength: 190-400nm; Sample feeding amount 5-20 μ l;
The secoiridoid glycoside content assaying method is as follows: the standard reference material of precision weighing 1mg is gentiopicrin, sweroside and sweroside respectively, adds dissolve with methanol respectively and is settled in the 2ml volumetric flask, is made into standard reference material solution;
High-efficient liquid phase chromatogram determining condition is as follows: C18 chromatographic column (150mm * 4.6mm, 5 μ m); 20 ℃ of column temperatures; Mobile phase: first alcohol and water, methanol and water volume ratio 80:20, isocratic elution time 30min; UV-detector detects wavelength: 190nm.Each standard reference material is respectively with 2,4,6,8,10 μ l sample introductions, record the high performance liquid chromatography peak area of each standard reference material, with each standard reference material peak area of gained is vertical coordinate, and each corresponding standard reference material content is abscissa drawing standard curve, calculates equation of linear regression;
Measure supplying test agent solution according to the high performance liquid chromatography experiment condition of standard substance then, the sample feeding amount is 5 μ l, obtain the peak area of the corresponding chromatographic peak of each standard reference material, record the content that supplies gentiopicrin, sweroside, sweroside in the test agent according to standard curve.
Beneficial effect: the present invention utilizes the soft ionization mass-spectrometric technique that the crude extract of Radix Gentianae is detected, and according to the number and the intensity of secoiridoid glycoside in the electron spray finger printing of the Radix Gentianae crude extract that obtains, the quality of Radix Gentianae is carried out preliminary assessment.This finger printing can clearly reflect because the difference of the place of production, secoiridoid glycoside kind that collecting season brought.The present invention considers that topmost drug activity composition is the Secoiridoid Glycosides chemical compound in the Radix Gentianae, and with gentiopicrin wherein, sweroside, three kinds of Secoiridoid Glycosides chemical compounds of sweroside are main, therefore the present invention with these three kinds of secoiridoid glycosides as standard reference material, pass through high-performance liquid chromatogram determination, obtain the standard curve and the equation of linear regression of each standard reference material, then to carrying out high-performance liquid chromatogram determination for test agent solution, obtain the peak area of the corresponding chromatographic peak of each standard reference material, record for gentiopicrin in the test agent according to standard curve, sweroside, the content of sweroside.
The sample pretreatment process of the method that the present invention provides is simple, the extraction efficiency height.The Electrospray Mass Spectrometry that utilizes the Chinese medicine Radix Gentianae extract is as finger printing, can clearly find out the Radix Gentianae mass discrepancy that the different places of production, Various Seasonal are gathered by the secoiridoid glycoside kind, in conjunction with the assay result of high performance liquid chromatography, can estimate again the quality of Chinese medicine Radix Gentianae to Lignanoids compounds in the Chinese medicine Radix Gentianae extract.
The specific embodiment
Embodiment 1:
(1) for the test agent formulations prepared from solutions
The Chinese medicine Radix Gentianae is pulverized, crossed 60 mesh sieves, take by weighing the Radix Gentianae 50mg that has pulverized and put in the 50ml conical flask, the adding concentration of volume percent is 50% methanol 5ml, supersound extraction 1 time, 20min/ time, 20 ℃ of supersound extraction temperature.Filter, merge said extracted liquid and be concentrated into 1ml, methanol constant volume shakes up to 10ml, is for test agent solution.
(2) the electron spray finger printing of confession test agent
Get for test agent solution, after 10 times of methanol dilutions, do the Electrospray Mass Spectrometry analysis.The Electrospray Mass Spectrometry experiment condition is as follows: the electron spray ionisation source, and spray voltage 3.5kV, 180 ℃ of capillary temperatures, injection pump sample introduction flow velocity 2 μ l/min flow; Sweep limits mass-to-charge ratio (m/z) 50-2000 utilizes the cation Electrospray Mass Spectrometry to confirm the kind of secoiridoid glycoside.Under the cation condition, in m/z 100-1000 scope, have m/z 379, m/z 381, and m/z 395, and m/z 735, and m/z 805, m/z 821 ions.
(3) secoiridoid glycoside assay
The high performance liquid chromatography experiment condition is as follows: C18 chromatographic column (150mm * 4.6mm, 5 μ m); 20 ℃ of column temperatures; Mobile phase: first alcohol and water, methanol and water volume ratio 80:20, isocratic elution time 30min; UV-detector detects wavelength: 190nm; Sample feeding amount 5 μ l.
The secoiridoid glycoside content assaying method is as follows: standard reference material gentiopicrin, sweroside, the sweroside of difference precision weighing 1mg, place the 2ml volumetric flask respectively, and add dissolve with methanol and be settled to scale, be made into standard reference material solution.High-performance liquid chromatogram determination, each standard reference material record the high performance liquid chromatography peak area of each standard reference material respectively with 2,4,6,8,10 μ l sample introductions.With each standard reference material peak area of gained is vertical coordinate, and each corresponding standard reference material content is abscissa drawing standard curve, calculates equation of linear regression.Measure supplying test agent solution according to the high performance liquid chromatography experiment condition of standard substance then, the sample feeding amount is 5 μ l,, obtain the peak area of the corresponding chromatographic peak of each standard reference material, record content according to standard curve for gentiopicrin, sweroside, sweroside in the test agent.
Embodiment 2:
(1) for the test agent formulations prepared from solutions
The Chinese medicine Radix Gentianae is pulverized, crossed 80 mesh sieves, take by weighing oneself the Radix Gentianae 200mg of pulverizing and put in the 50ml conical flask, adding concentration of volume percent is 100% methanol 20ml, supersound extraction 3 times, 40min/ time, 50 ℃ of supersound extraction temperature.Filter, merge said extracted liquid and be concentrated into 2ml, methanol constant volume shakes up to 10ml, is for test agent solution.
(2) the electron spray finger printing of confession test agent
Get for test agent solution, after 10 times of methanol dilutions, do the Electrospray Mass Spectrometry analysis.The Electrospray Mass Spectrometry experiment condition is as follows: the electron spray ionisation source, and spray voltage 5.5kV, 220 ℃ of capillary temperatures, injection pump sample introduction flow velocity 8 μ l/min flow; Sweep limits mass-to-charge ratio (m/z) 50-2000 utilizes the cation Electrospray Mass Spectrometry to confirm the kind of secoiridoid glycoside.Under the cation condition, in m/z 100-1000 scope, have m/z 379, m/z 381, and m/z 395, and m/z 735, and m/z 805, m/z 821 ions.
(3) secoiridoid glycoside assay
The high performance liquid chromatography experiment condition is as follows: C18 chromatographic column (150mm * 4.6mm, 5 μ m); 35 ℃ of column temperatures; Mobile phase: first alcohol and water, methanol and water volume ratio 30:70, isocratic elution time 60min; UV-detector detects wavelength: 400nm; Sample feeding amount 20 μ l.
The secoiridoid glycoside content assaying method is with embodiment 1
Embodiment 3:
(1) for the test agent formulations prepared from solutions
The Chinese medicine Radix Gentianae is pulverized, crossed 70 mesh sieves, take by weighing the Radix Gentianae 150mg that has pulverized and put in the 50ml conical flask, adding concentration of volume percent is 75% methanol 15ml, supersound extraction 2 times, 30min/ time, 35 ℃ of supersound extraction temperature.Filter, merge said extracted liquid and be concentrated into 1.5ml, methanol constant volume shakes up to 10ml, is for test agent solution.
(2) the electron spray finger printing of confession test agent
Get for test agent solution, after 10 times of methanol dilutions, do the Electrospray Mass Spectrometry analysis.The Electrospray Mass Spectrometry experiment condition is as follows: the electron spray ionisation source, and spray voltage 4.5kV, 200 ℃ of capillary temperatures, injection pump sample introduction flow velocity 6 μ l/min flow; Sweep limits mass-to-charge ratio (m/z) 50-2000 utilizes the cation Electrospray Mass Spectrometry to confirm the kind of secoiridoid glycoside.Under the cation condition, in m/z 100-1000 scope, have m/z 379, m/z 381, and m/z 395, and m/z 735, and m/z 805, m/z 821 ions.
(3) secoiridoid glycoside assay
The high performance liquid chromatography experiment condition is as follows: C18 chromatographic column (150mm * 4.6mm, 5 μ m); 30 ℃ of column temperatures; Mobile phase: first alcohol and water, methanol and water volume ratio 80:20-30:70, gradient elution time 45min; UV-detector detects wavelength: 300nm; Sample feeding amount 15 μ l.
The secoiridoid glycoside content assaying method is with embodiment 1
Embodiment 4:
(1) for the test agent formulations prepared from solutions
The Chinese medicine Radix Gentianae is pulverized, crossed 60 mesh sieves, take by weighing the Radix Gentianae 125mg that has pulverized and put in the 50ml conical flask, adding concentration of volume percent is 100% methanol 10ml, supersound extraction 2 times, 30min/ time, 25 ℃ of supersound extraction temperature.Filter, merge said extracted liquid and be concentrated into 1ml, methanol constant volume shakes up to 10ml, is for test agent solution.
(2) the electron spray finger printing of confession test agent
Get for test agent solution, after 10 times of methanol dilutions, do the Electrospray Mass Spectrometry analysis.The Electrospray Mass Spectrometry experiment condition is as follows: the electron spray ionisation source, and spray voltage 4.0kV, 190 ℃ of capillary temperatures, injection pump sample introduction flow velocity 5 μ l/min flow; Sweep limits mass-to-charge ratio (m/z) 50-2000 utilizes the cation Electrospray Mass Spectrometry to confirm the kind of secoiridoid glycoside.Under the cation condition, in m/z 100-1000 scope, have m/z 379, m/z 381, and m/z 395, and m/z 735, and m/z 805, m/z 821 ions.
(3) secoiridoid glycoside assay
The high performance liquid chromatography experiment condition is as follows: C18 chromatographic column (150mm * 4.6mm, 5 μ m); 30 ℃ of column temperatures; Mobile phase: first alcohol and water, methanol and water volume ratio 55:45-30:70, gradient elution time 60min; UV-detector detects wavelength: 260nm; Sample feeding amount 10 μ l.
The secoiridoid glycoside content assaying method is with embodiment 1
Embodiment 5:
(1) for the test agent formulations prepared from solutions
The Chinese medicine Radix Gentianae is pulverized, crossed 70 mesh sieves, take by weighing the Radix Gentianae 100mg that has pulverized and put in the 50ml conical flask, adding concentration of volume percent is 50% methanol 20ml, supersound extraction 3 times, 20min/ time, 40 ℃ of supersound extraction temperature.Filter, merge said extracted liquid and be concentrated into 2ml, methanol constant volume shakes up to 10ml, is for test agent solution.
(2) the electron spray finger printing of confession test agent
Get for test agent solution, after 10 times of methanol dilutions, do the Electrospray Mass Spectrometry analysis.The Electrospray Mass Spectrometry experiment condition is as follows: the electron spray ionisation source, and spray voltage 5.0kV, 210 ℃ of capillary temperatures, injection pump sample introduction flow velocity 4 μ l/min flow; Sweep limits mass-to-charge ratio (m/z) 50-2000 utilizes the cation Electrospray Mass Spectrometry to confirm the kind of secoiridoid glycoside.Under the cation condition, in m/z 100-1000 scope, have m/z 379, m/z 381, and m/z 395, and m/z 735, and m/z 805, m/z 821 ions.
(3) secoiridoid glycoside assay
The high performance liquid chromatography experiment condition is as follows: C18 chromatographic column (150mm * 4.6mm, 5 μ m); 25 ℃ of column temperatures; Mobile phase: first alcohol and water, methanol and water volume ratio 80:20-55:45, gradient elution time 50min; UV-detector detects wavelength: 350nm; Sample feeding amount 10 μ l.
The secoiridoid glycoside content assaying method is with embodiment 1
Embodiment 6:
(1) for the test agent formulations prepared from solutions
The Chinese medicine Radix Gentianae is pulverized, crossed 80 mesh sieves, take by weighing the Radix Gentianae 175mg that has pulverized and put in the 50ml conical flask, adding concentration of volume percent is 100% methanol 15ml, supersound extraction 3 times, 20min/ time, 40 ℃ of supersound extraction temperature.Filter, merge said extracted liquid and be concentrated into 1.5ml, methanol constant volume shakes up to 10ml, is for test agent solution.
(2) the electron spray finger printing of confession test agent
Get for test agent solution, after 10 times of methanol dilutions, do the Electrospray Mass Spectrometry analysis.The Electrospray Mass Spectrometry experiment condition is as follows: the electron spray ionisation source, and spray voltage 4.0kV, 160 ℃ of capillary temperatures, injection pump sample introduction flow velocity 7 μ l/min flow; Sweep limits mass-to-charge ratio (m/z) 50-2000 utilizes the cation Electrospray Mass Spectrometry to confirm the kind of secoiridoid glycoside.Under the cation condition, in m/z 100-1000 scope, have m/z 379, m/z 381, and m/z 395, and m/z 735, and m/z 805, m/z 821 ions.
(3) secoiridoid glycoside assay
The high performance liquid chromatography experiment condition is as follows: C18 chromatographic column (150mm * 4.6mm, 5 μ m); 30 ℃ of column temperatures; Mobile phase: first alcohol and water, methanol and water volume ratio 55:45, isocratic elution time 45min; UV-detector detects wavelength: 280nm; Sample feeding amount 20 μ l.
The secoiridoid glycoside content assaying method is with embodiment 1.
Claims (1)
1. quality detection method of Chinese herb gentian, its spy just is that step and condition are as follows: the Chinese medicine Radix Gentianae was pulverized the 60-80 mesh sieve, take by weighing the Radix Gentianae 50-200mg that has pulverized and put in the 50ml conical flask, the methanol that with the concentration of volume percent is 50%-100% adds methanol 5-20ml as solvent, supersound extraction 1-3 time, 20-40min/ time, 20-50 ℃ of supersound extraction temperature filtered, merge said extracted liquid and be concentrated into 1-2ml, methanol constant volume shakes up to 10ml, is for test agent solution;
The electron spray finger printing of sample obtains as follows: get 50-100 μ L for test agent solution, after 10 times of methanol dilutions, do the Electrospray Mass Spectrometry analysis; The Electrospray Mass Spectrometry experiment condition is as follows: the electron spray ionisation source, and spray voltage 3.5-5.5kV, capillary temperature 180-220 ℃, injection pump sample introduction flow velocity 2-8 μ l/min flows; Sweep limits mass-to-charge ratio (m/z) 50-2000 utilizes the cation Electrospray Mass Spectrometry to confirm the kind of secoiridoid glycoside, under the cation condition, in m/z 100-1000 scope, have m/z 379, m/z 381, and m/z 395, m/z 735, and m/z 805, m/z 821 ions;
The high-efficient liquid phase chromatogram technology condition is as follows: C18 chromatographic column condition is 150mm * 4.6mm, 5 μ m, column temperature 20-35 ℃; Mobile phase is the first alcohol and water, methanol and water volume ratio 80:20-30:70, elution time 30-60min; UV-detector detects wavelength: 190-400nm; Sample feeding amount 5-20 μ l;
The secoiridoid glycoside content assaying method is as follows: the standard reference material of precision weighing 1mg is gentiopicrin, sweroside and sweroside respectively, adds dissolve with methanol respectively and is settled in the 2ml volumetric flask, is made into standard reference material solution;
High-efficient liquid phase chromatogram determining condition is as follows: C18 chromatographic column (150mm * 4.6mm, 5 μ m); 20 ℃ of column temperatures; Mobile phase: first alcohol and water, methanol and water volume ratio 80:20, isocratic elution time 30min; UV-detector detects wavelength: 190nm; Each standard reference material is respectively with 2,4,6,8,10 μ l sample introductions, record the high performance liquid chromatography peak area of each standard reference material, with each standard reference material peak area of gained is vertical coordinate, and each corresponding standard reference material content is abscissa drawing standard curve, calculates equation of linear regression;
Measure supplying test agent solution according to the high performance liquid chromatography experiment condition of standard substance then, the sample feeding amount is 5 μ l, obtain the peak area of the corresponding chromatographic peak of each standard reference material, record the content that supplies gentiopicrin, sweroside, sweroside in the test agent according to standard curve.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103007389A (en) * | 2012-12-14 | 2013-04-03 | 南京航空航天大学 | Vein infusion device and system based on fuzzy PI (Proportional Integral) control |
| CN105467033A (en) * | 2015-12-15 | 2016-04-06 | 河北科技大学 | Method for building swertia pseudochinensis medicine material fingerprint spectrum and fingerprint spectrum and application thereof |
| CN108169345A (en) * | 2017-11-10 | 2018-06-15 | 内蒙古医科大学 | Anaesthetic radix gentiane dahuvicae fingerprint and quality evaluating method |
| CN109358136A (en) * | 2018-12-21 | 2019-02-19 | 广东方制药有限公司 | A kind of identification and the differentiating method of Chinese medicine rough gentian and Gentiana rigescens |
| CN112578049A (en) * | 2020-12-10 | 2021-03-30 | 新疆医科大学第一附属医院 | Method for detecting iridoid glycoside in gentianella virginiana by UPLC-MS/MS (ultra Performance liquid chromatography-Mass Spectrometry/Mass Spectrometry) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101306139A (en) * | 2008-06-26 | 2008-11-19 | 广州奇星药业有限公司 | Quality control method of Biyan Qingdu granule |
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- 2009-04-27 CN CN 200910066875 patent/CN101530463B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103007389A (en) * | 2012-12-14 | 2013-04-03 | 南京航空航天大学 | Vein infusion device and system based on fuzzy PI (Proportional Integral) control |
| CN105467033A (en) * | 2015-12-15 | 2016-04-06 | 河北科技大学 | Method for building swertia pseudochinensis medicine material fingerprint spectrum and fingerprint spectrum and application thereof |
| CN108169345A (en) * | 2017-11-10 | 2018-06-15 | 内蒙古医科大学 | Anaesthetic radix gentiane dahuvicae fingerprint and quality evaluating method |
| CN109358136A (en) * | 2018-12-21 | 2019-02-19 | 广东方制药有限公司 | A kind of identification and the differentiating method of Chinese medicine rough gentian and Gentiana rigescens |
| CN112578049A (en) * | 2020-12-10 | 2021-03-30 | 新疆医科大学第一附属医院 | Method for detecting iridoid glycoside in gentianella virginiana by UPLC-MS/MS (ultra Performance liquid chromatography-Mass Spectrometry/Mass Spectrometry) |
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Effective date of registration: 20130930 Address after: Changzhou City, Jiangsu province Hehai road 213000 No. 9 Patentee after: Changzhou Institute of Energy Storage Materials & Devices Address before: 130022 Changchun people's street, Jilin, No. 5625 Patentee before: Changchun Institue of Applied Chemistry, Chinese Academy of Sciences |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130102 Termination date: 20210427 |