CN106053626B - The method for quickly measuring echinacoside and acteoside active constituent in Herba Cistanches - Google Patents
The method for quickly measuring echinacoside and acteoside active constituent in Herba Cistanches Download PDFInfo
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- CN106053626B CN106053626B CN201610319728.XA CN201610319728A CN106053626B CN 106053626 B CN106053626 B CN 106053626B CN 201610319728 A CN201610319728 A CN 201610319728A CN 106053626 B CN106053626 B CN 106053626B
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- acteoside
- echinacoside
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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Abstract
The present invention relates to a kind of methods of echinacoside and acteoside active constituent in quick measurement Herba Cistanches, this method quantitative determines two kinds of echinacoside, acteoside active constituents in Herba Cistanches using ultra performance liquid chromatography mass spectrometric hyphenated technique, it is tested through methodological study, confirm this method, analyze speed is faster（Test is completed in 5 minutes）, high sensitivity, favorable reproducibility are the more rapidly effective means for measuring two kinds of active component contents in Herba Cistanches simultaneously.
Description
Technical field
The present invention relates to a kind of methods of echinacoside and acteoside active constituent in quick measurement Herba Cistanches, especially
Relating to the use of ultra performance liquid chromatography-mass spectrometric hyphenated technique, quickly analysis measures echinacoside, verbascose in Herba Cistanches simultaneously
The method of glycosides active component content.
Background technology
Herba Cistanches (Cistanche deserticola Ma) are Orobanchaceae Orobanchaceae Cistanche deserticolas
Cistanche Hoffmg.et Link, medicinal effects are dry meat stem, and there is kidney-replenishing, benefiting essence-blood to relax bowel it
Effect, main effective component are benzyl carbinol glycoside compound.Have document report detection Herba Cistanches in two kinds mainly at
Divide but run time is relatively long, longest to need separate two components within 60 minutes, this method uses mass detector,
And in chromatographic column, flow velocity is all different from the document of following report in run time, run time is especially foreshortened to 5 points
Clock.
In Chinese Pharmaceutical Journal 39 (10) in 2004:It appears in the newspapers and HPLC while measuring in Herba Cistanches medicinal material loose in 740-741
The content (Zhang Siju) of fruit chrysanthemum glycosides and acteoside, YMC-Pack ODS-A (5 μm, 25*4.6mm) chromatographic column used, 30 DEG C
Column temperature, CH3CN-MeOH-1%HAc (10:15:75) it is mobile phase, flow velocity 0.7mL/min, Detection wavelength 334nm, run time
40 minutes.CHINA JOURNAL OF CHINESE MATERIA MEDICA 2005,30 (11)：Echinacoside and verbascose glycosides in the Cistanche tubulosa reported in 839-841
Assay (Chen Min), chromatographic column used be Agilent Eclipse DB-C18 (4.6*250mm, 5 μm), column temperature, flowing
Mutually and Detection wavelength has no improvement, and only flow velocity is changed to 0.6mL/min, run time 25 minutes.Chinese pharmacy in 2007 is miscellaneous
There is a report HPLC to measure pine in desert cistanche oral liquid as cathartics in will Shimadzu cup whole nation Pharmaceutical Analysis best paper competition exchanging meeting
The content (Liu Lansheng) of fruit chrysanthemum glycosides and acteoside, Hypersil C18 (4.6mm × 250mm, 5 μm)；Mobile phase：Acetonitrile-
One 1% acetum (10 of methanol:l0:80)；Column temperature, Detection wavelength is with the first two year document report without improvement；Flow velocity is changed to 1mL/
min；Run time is 40 minutes.
2009 medicine Leader 28 (2):The high effective liquid chromatography for measuring compound Herba Cistanches oral solution reported in 231-232
Echinacoside and acteoside content (Kang Airong), this method use YMC-Pack ODS-A (6.0mm × 150mm, 5 μm) color
Column is composed, 35 DEG C of column temperatures, mobile phase is -0.2% formic acid solution of methanol, gradient elution, and flow velocity is increased to 1.0mL/min, detects wave
Long 334nm is constant, and run time is 30 minutes.The middle co-occurrence in the same year is for medicinal application 15：It the HPLC that is reported in 14-16 while surveying
The content (Huo Yanxian) of echinacoside and acteoside uses high performance liquid chromatography in the fixed strong prebiotic ball of member, with YMC-
PackODS-A (250mm × 4.6mm, 5 μm) chromatographic column is stationary phase, -1% acetic acid aqueous solution (10 of acetonitrile-methanol:13:77) it is
Mobile phase, column temperature are 30 DEG C, and flow velocity and Detection wavelength are all unchanged, only run time 45 minutes.
In Chinese herbal medicine 41 (12) in 2010：The wide intestines Liqi Decoction of high effective liquid chromatography for measuring reported in 1994-1995
Middle echinacoside and acteoside (Zhang Yan), this method use chromatographic column for Agilent C18 (250mm × 4.6mm, 5 μm),
Mobile phase is that -1% glacial acetic acid of acetonitrile carries out gradient elution, and it is 40 DEG C that column temperature, which is increased to, and flow rate detection wavelength is not any change still,
Run time is 35 minutes.
Chinese patent drug 35 (12) in 2013：The HPLC methods measurement reported in 2649-2653 exempts from catechin, table in numbness Kang Sheng Pill
Theine, echinacoside and acteoside (Hou Ying), Hypersil C18 chromatographic columns (4.6mm × 150mm, 5 μm), flow velocity is still
1.0mL/min, mobile phase A are l% glacial acetic acid solutions, and Mobile phase B is acetonitrile-methanol (1: 4), Detection wavelength 330nm, when operation
Between 8 minutes.
Chinese pharmacists, 2014 (8)：The HPLC methods reported in 1336-1338 measure in strong kidney heart tonifying capsule echinacoside and
The content (Lu Caiyang) of acteoside, using chromatographic column Shim-pack VP-ODS C18, mobile phase is -0.1% first of methanol
Acid solution carries out gradient elution, and Detection wavelength is that 330nm is constant, and flow velocity is the same as last year document report and unchanged, column temperature 28
℃.Run time 35 minutes.Treasure's traditional Chinese medical science traditional Chinese medicines 5 when the same year：The Cistanche tubulosa difference growth time reported in 1191-1193 and
The active constituent content analysis (Yang Taixin) at position, chromatographic column Agilent Zorbax SB C18 (150mm × 4.6mm, 5 μm)；
Mobile phase:- 0.1% formic acid gradient of methanol elutes, and flow rate detection wavelength is the same as the same year document indistinction, 35 DEG C of column temperature, run time
60 minutes.
In the detection method that 2015 have 5 document reports similar, World Science technology-traditional Chinese medicine modernizes 17 (3)：
HPLC methods in 609-613 measure the content of echinacoside, acteoside, different acteoside in Cistanchis glycosides capsule simultaneously
(Yang Su DS), Waters C18 chromatographic columns (4.6mm × 150mm, 5 μm), mobile phase:- 0.1% formic acid solution gradient of methanol is washed
It is de-；Flow velocity still uses 1.0mL/min；Detection wavelength adopts the 330nm of document report in 2013；30 DEG C of run times 50 of column temperature
Minute.43 (33) in Agriculture of Anhui science：The HPLC of 171-173 reports measures echinacoside and verbascose in Herba Cistanches micro mist
The content (Tian Yubiao) of glycosides, Waters C18 columns (4.6mm × 250mm, 5 μm) are flowing with -0.1% aqueous formic acid of methanol
Phase gradient elutes；Flow velocity, detection involve column temperature and are not any change, and run time is 40 minutes；Chinese pharmacists 8, in 1404-1406
The one of report surveys and comments 2 kinds of active constituent contents (appointing disabled soldier) in method measurement Herba Cistanches more, Ultimate-C18 (250mm ×
4.6mm, 5 μm)；Mobile phase:- 0.1% formic acid (B) of methanol (A), gradient elution；Flow velocity, Detection wavelength and column temperature are unchanged；
Run time 45 minutes.
The same year pharmacopeia is updated to using octadecylsilane chemically bonded silica as filler；Using methanol as mobile phase A, with 0.1%
Formic acid solution is Mobile phase B, gradient elution；Detection wavelength is 330nm, run time 27 minutes.
Invention content
The object of the present invention is to provide a kind of quickly analyses to measure echinacoside and acteoside activity in Herba Cistanches
The method of ingredient.This method is using ultra performance liquid chromatography-mass spectrometric hyphenated technique to echinacoside, acteoside in Herba Cistanches
Two kinds of active constituents are quantitative determined, and are tested through methodological study, confirm that this method, analyze speed faster (are completed in 5 minutes
Test), high sensitivity, favorable reproducibility are the more rapidly effective means for measuring two kinds of active component contents in Herba Cistanches simultaneously.
The method of echinacoside and acteoside active constituent in a kind of quick measurement Herba Cistanches of the present invention, profit
With High Performance Liquid Chromatography/Mass Spectrometry condition, concrete operations follow these steps to carry out：
A, ultra performance liquid chromatography condition：Chromatographic column：Hypersil GOLD,C18 100×2.1mm,1.9μm；Mobile phase
Percent by volume is A-0.1% aqueous formic acids, B- methanol；Temporally 0min, 3.0min, 4.0min, 4.1min, 5.0min,
Respectively with a concentration of 80%, 28%, 28%, 80%, 80% A-0.1% aqueous formic acids and a concentration of 20%, 72%,
72%, 20%, 20% methanol solution carries out gradient elution, flow velocity：0.2mL/min；Column temperature：Room temperature；Sample size：5μL；
B, Mass Spectrometry Conditions：Ion source voltage：-3000v；Ion source temperature：200℃；Sheath gas：35arb；Assist gas：8arb；
Ion transfer capillary temperature：350℃；Type ion source：Electric spray ion source, acteoside retention time 3.7 minutes are female
Ion m/z 623.154, fragments characteristic ion 162.229 and 461.374 (for quota ion)；Echinacoside retention time is
3.3 minutes, parent ion m/z 785.189, fragments characteristic ion was m/z 477.305 and 623.471 (for quota ion)；
C, the preparation of reference substance solution：Precision weighs each component 1.00mg, is settled to 1mL with methanol dissolving respectively, as
Reference substance solution storing solution；
D, the preparation of sample solution：With reference to Chinese Pharmacopoeia 2015 editions；
E, the drafting of standard curve：Precision pipettes two kinds of active constituents of echinacoside and acteoside, is with diluent
Volume ratio 80:20 water:Methanol dilutes 10 respectively3,5×103,104,5×104,105,5×105Times, obtain mixed mark solution；It presses
Chromatographic condition carries out super ultra performance liquid chromatography-mass spectral analysis；Regression analysis is carried out to peak area with concentration, obtains each component standard
Curve calculates regression equation；
F, precision test：6 needle of continuous sample introduction measures peak area RSD 0.59%-0.79%, relative retention time
RSD0.11%-0.13%；
G, repetitive test：Herba Cistanches powder 1g is taken, it is totally 7 parts, accurately weighed, it is extracted and is analyzed by step d；
H, stability test：Take with portion test solution in step d, respectively at 0,2,4,6,8h sample introductions, measure wherein
The content of echinacoside and acteoside, and calculate RSD values；
I, sample size measures：Accurate pipette samples prepare liquid carries out ultra performance liquid chromatography-mass spectrum point by chromatographic condition
Analysis, and bring peak area into standard curve, calculate separately the content of echinacoside and acteoside.
Description of the drawings
Fig. 1 is the spectrogram of sample in standard specimen of the present invention, wherein RT:3.70 be Herba Cistanches active ingredient acteoside, RT:
3.26 be Herba Cistanches active ingredient echinacoside；
Fig. 2 is the spectrogram in present example sample, wherein RT:3.70 be Herba Cistanches active ingredient acteoside, RT:
3.27 be Herba Cistanches active ingredient echinacoside.
Specific implementation mode
Embodiment
The method of echinacoside and acteoside active constituent in a kind of quick measurement Herba Cistanches of the present invention, tool
Gymnastics follows these steps to carry out：
Instrument condition：
Ultra performance liquid chromatography condition：Chromatographic column：Hypersil GOLD,C18 100×2.1mm,1.9μm；Mobile phase：
A-0.1% aqueous formic acids；B- methanol；Elution program is as follows：0-3 minutes, A 80%-28%；3-4 minutes, A 28%；4.0-
4.1 minutes A 28%-80%；4.1-5.0 minute A 80%；Flow velocity：0.2mL/min；Column temperature：Room temperature；Sample size：5μL；
Mass Spectrometry Conditions：Ion source voltage：-3000v；Ion source temperature：200℃；Sheath gas：35arb；Assist gas：8arb；From
Sub- transfer capillary temperature：350℃；Electric spray ion source
The preparation of reference substance solution：Precision weighs each component 1.00mg, 1mL is settled to methanol dissolving respectively, as right
According to product solution storing solution；
The preparation of sample solution：With reference to Chinese Pharmacopoeia 2015 editions；
The drafting of standard curve：Precision pipettes two kinds of active constituents of echinacoside and acteoside, is body with diluent
Product ratio 80:20 water:Methanol dilutes 10 respectively3,5×103,104,5×104,105,5×105Times, obtain mixed mark solution；By color
Spectral condition carries out super ultra performance liquid chromatography-mass spectral analysis；Regression analysis is carried out to peak area with concentration, it is bent to obtain each component standard
Line calculates regression equation；
Precision test：6 needle of continuous sample introduction measures peak area RSD 0.59%-0.79%, relative retention time
RSD0.11%-0.13%；It is 97.64%-107.36%, relative standard deviation RSD 1.56%-3.88% to measure the rate of recovery；
Repetitive test：Herba Cistanches powder about 1g is taken, it is totally 7 parts, accurately weighed, by the preparation of sample solution (with reference to China
Pharmacopeia 2015 editions) it extracts and analyzes, result is：
Stability test：Take with portion test solution in repetitive test, respectively at 0,2,4,6,8h sample introductions, measure it
The content of middle echinacoside and acteoside, and it is respectively 0.6%, 0.5% to calculate RSD values；
Sample size measures：Accurate pipette samples prepare liquid carries out ultra performance liquid chromatography-mass spectrum point by chromatographic condition
Analysis, and bring peak area into standard curve, the content for calculating separately echinacoside is 15.08-18.96mg/g, acteoside
Content be 5.06-5.48mg/g.
Claims (1)
1. a kind of method of echinacoside and acteoside active constituent in quick measurement Herba Cistanches, it is characterised in that utilize super
High Performance Liquid Chromatography/Mass Spectrometry condition, concrete operations follow these steps to carry out：
A, ultra performance liquid chromatography condition：Chromatographic column： Hypersil GOLD, C18 100×2.1mm,1.9μm；Mobile phase body
Product percentage is A-0.1% aqueous formic acids, B- methanol；Temporally 0min, 3.0min, 4.0min, 4.1min, 5.0min,
Respectively with a concentration of 80%, 28%, 28%, 80%, 80% A-0.1% aqueous formic acids and a concentration of 20%, 72%, 72%, 20%, 20%
Methanol solution carry out gradient elution, flow velocity：0.2mL/min；Column temperature：Room temperature；Sample size：5μL；
B, Mass Spectrometry Conditions：Ion source voltage：-3000v；Ion source temperature：200℃；Sheath gas：35arb；Assist gas：8arb；Ion
Transfer capillary temperature：350℃；Type ion source：Electric spray ion source, acteoside retention time 3.7 minutes, parent ion
M/z 623.154, fragments characteristic ion 162.229 and 461.374；Echinacoside retention time is 3.3 minutes, parent ion m/z
785.189, fragments characteristic ion is m/z 477.305 and 623.471；
C, the preparation of reference substance solution：Precision weighs each component 1.00mg, is settled to 1mL with methanol dissolving respectively, as a contrast
Product solution storing solution；
D, the preparation of sample solution：Herba Cistanches powder 1g is taken, No. four sieves are crossed, it is accurately weighed, it sets in 100mL brown volumetric flasks, essence
50% methanol 50mL of close addition, close plug shake up, weighed weight, impregnate 30 minutes, are ultrasonically treated 40 minutes, power 250W, frequency
35kHz is let cool, then weighed weight, is added 50% methanol to supply the weight of less loss, is shaken up, and is stood, is taken supernatant, is filtered, is taken continuous filter
Liquid to get；
E, the drafting of standard curve：Precision pipettes two kinds of active constituents of echinacoside and acteoside, is volume with diluent
Than 80:20 water:Methanol dilutes 10 respectively3,5×103,104,5×104,105,5×105Times, obtain mixed mark solution；By chromatography
Condition carries out ultra performance liquid chromatography-mass spectral analysis；Regression analysis is carried out to peak area with concentration, obtains each component standard curve,
Calculate regression equation；
F, precision test：6 needle of continuous sample introduction measures peak area RSD 0.59%-0.79%, relative retention time RSD 0.11%-
0.13%；
G, repetitive test：Herba Cistanches powder 1g is taken, it is totally 7 parts, accurately weighed, it is extracted and is analyzed by step d；
H, stability test：Take with portion sample solution in step d, respectively at 0,2,4,6,8h sample introductions, measure wherein Echinacea purpurea
The content of glycosides and acteoside, and calculate RSD values；
I, sample size measures：Accurate pipette samples solution carries out ultra performance liquid chromatography-mass spectral analysis by chromatographic condition, and
It brings peak area into standard curve, calculates separately the content of echinacoside and acteoside.
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| CN109507319A (en) * | 2018-11-20 | 2019-03-22 | 中国科学院新疆生态与地理研究所 | A kind of method of resveratrol activity component content in quick measurement tree peony fruit pod |
| CN109991328B (en) * | 2019-04-04 | 2022-04-22 | 西安医学院 | Quality evaluation method for one-test-multiple evaluation of affine cudweed |
| CN110092805B (en) * | 2019-06-12 | 2020-11-13 | 劲牌有限公司 | Method for extracting echinacoside and verbascoside from cistanche |
| CN112630327B (en) * | 2020-12-03 | 2023-04-07 | 武汉职业技术学院 | Quick detection method for active ingredients of cistanche |
| CN115128200B (en) * | 2022-07-26 | 2024-01-19 | 吉首大学 | HPLC quality detection method for paulownia tomentosa leaves |
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| CN104569217A (en) * | 2013-10-12 | 2015-04-29 | 广州奇绩医药科技有限公司 | Method for establishing Jinrong Xiaopi granule fingerprint |
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| CN104569217A (en) * | 2013-10-12 | 2015-04-29 | 广州奇绩医药科技有限公司 | Method for establishing Jinrong Xiaopi granule fingerprint |
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