CN105866285A - Method for measuring mangiferin and bergenin in heat-clearing cough-relieving syrup in manner of liquid mass spectrum serial connection - Google Patents
Method for measuring mangiferin and bergenin in heat-clearing cough-relieving syrup in manner of liquid mass spectrum serial connection Download PDFInfo
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- CN105866285A CN105866285A CN201610263368.6A CN201610263368A CN105866285A CN 105866285 A CN105866285 A CN 105866285A CN 201610263368 A CN201610263368 A CN 201610263368A CN 105866285 A CN105866285 A CN 105866285A
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- mass spectrum
- liquid mass
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- bergenin
- mangiferin
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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
-
- 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
Abstract
The invention provides a method for measuring mangiferin and bergenin in heat-clearing cough-relieving syrup in a manner of liquid mass spectrum serial connection. The invention aims to provide the method for measuring mangiferin and bergenin in heat-clearing cough-relieving syrup in the manner of liquid mass spectrum serial connection, which has the advantages of simple detection and high detection result accuracy. The method comprises the following steps: precisely taking 1ml sample; putting into a 10mL extraction pool; statically extracting the sample for 3min at 60 DEG C with methyl alcohol; repeatedly extracting for 2 times; after completing extraction, using methyl alcohol for keeping the constant volume of the extracting solution at 20mL; sucking the extracting solution into a 1mL centrifugal tube; swirling for 2min; centrifuging for 3min at the speed of 15000r/min; and taking the supernate and performing chromatographic analysis. The method belongs to the technical field of chemical detection.
Description
Technical field
The invention provides a kind of liquid mass spectrum series connection and measure chimonin and rock in reducing fever relieving cough syrup
The method of Chinese cabbage element；Belong to technical field of chemical detection.
Background technology
Reducing fever relieving cough syrup is Semen Lepidii (Semen Descurainiae), Herba Ardisiae Japonicae, Herba Houttuyniae, Herba Schizonepetae, Radix Peucedani, Semen Castaneae
Shell, Pumex totally 8 taste medicine composition, has the effect of heat clearing away town expectorant, applies it to control clinically
Treat flu the disease such as pharyngitis, cough due to lung-heat, it was reported that reducing fever relieving cough syrup to staphylococcus aureus,
The common antibacterial of the respiratory tract infection such as beta hemolytic streptococcus, streptococcus pneumoniae has different journey
The inhibitory action of degree；The production technology recording this medicine according to pharmacopeia is " boiling two
Secondary, 2 hours for the first time, 1.5 hours for the second time, filter, merging filtrate is also concentrated into about
650ml, stands, and filters, and filtrate is standby.Separately take sucrose 450g add water boil in right amount molten
Solve, add above-mentioned concentrated solution, benzoic acid 2.5g, ethyl hydroxybenzoate 0.5g (benzoic acid and oxybenzene
Ethyl ester dissolves with a small amount of ethanol) and essence is in right amount, adds water to 1000ml, stirs evenly, i.e.
", in real work, find to advise in pharmacopeia on sample chromatogram figure according to official method
There will be identical with gradient condition chromatograph environment baseline up drift under fixed isocratic chromatograph environment
Situation, affect the integration of this composition of sample, easily the quality of sample judged by accident, and
Identical chromatographic condition the most not this situation in reference substance chromatograph.In the technique of this sample
Because the acids such as anticorrosion needs to add a certain amount of benzoic acid, benzoic acid hangover is serious
It it is the main cause causing this impact.
Summary of the invention
It is an object of the invention to provide a kind of detection method simple, testing result degree of accuracy is high
The series connection of liquid mass spectrum measure chimonin and the method for Bergeninum in reducing fever relieving cough syrup.
The series connection of a kind of liquid mass spectrum measures chimonin and the side of Bergeninum in reducing fever relieving cough syrup
Method, described detection method comprises the steps: successively
Precision measures this product 1ml, is placed in 10mL abstraction pool, with methanol to sample in temperature
Spend 60 DEG C, static extraction 3min, repeats to extract 2 times, by extracting solution first after having extracted
Alcohol is settled to 20mL, draws 1mL in centrifuge tube, whirlpool 2min, 15000r/min from
Heart 3min, takes supernatant and carries out chromatography；
Described chromatographic condition is as follows:
Chromatographic condition is as follows:
Chromatographic column: Kromasil-C18 post, 50mm × 4.6mm × 5mm；
Mobile phase methanol-acetonitrile-1mmol/L ammonium acetate solution, uses gradient elution；
Flow velocity: 1mL min-1；
Column temperature: 35 DEG C；
Sample size 1 μ L；
Mass Spectrometry Conditions:
Ion source: electric spray ion source；
Source injection electric cation 5 500V；Anion-4 500V；
Ion source temperature: 350 DEG C；
Whole process is passed through nitrogen.
Further, above-mentioned a kind of liquid mass spectrum series connection measures chimonin in reducing fever relieving cough syrup
With the method for Bergeninum, described gradient elution program is as follows: 0～1min, 85%～
45%A, 10%B, 5%～45%C；1～2.5min, 45%A, 10%B, 45%C；
2.5～7min, 45%～31%A, 10%～14%B, 45%C；7～12min, 31%～
0%A, 14%～50%B, 50%C；12～15min, 0%～85%A, 50%～
10%B, 50%～5%C；3min is balanced under 85%A, 10%B, 5%C.
Compared with prior art, the technical scheme that the present invention provides uses liquid chromatograph associating matter
Spectrum, the method for gradient elution, praeruptorin A element, the party in detection reducing fever relieving cough syrup
Method is simple to operate, favorable reproducibility, high-specificity, and chromatographic peak separating degree is good, is conducive to controlling
The quality of product.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the claim of the present invention is done the most in detail
Illustrate, but do not constitute any limitation of the invention, any in the claims in the present invention protection
The amendment of the limited number of time that scope is made, still within the claims of the present invention.
Involved in the present invention to percentage composition concentration, in addition to specified otherwise, solute is liquid
Be volumetric concentration, solute be solid be mass concentration.
Embodiment 1
The series connection of a kind of liquid mass spectrum measures chimonin and the side of Bergeninum in reducing fever relieving cough syrup
Method, described detection method comprises the steps: successively
Precision measures this product 1ml, is placed in 10mL abstraction pool, with methanol to sample in temperature
Spend 60 DEG C, static extraction 3min, repeats to extract 2 times, by extracting solution first after having extracted
Alcohol is settled to 20mL, draws 1mL in centrifuge tube, whirlpool 2min, 15000r/min from
Heart 3min, takes supernatant and carries out chromatography；
Described chromatographic condition is as follows:
Chromatographic condition is as follows:
Chromatographic column: Kromasil-C18 post, 50mm × 4.6mm × 5mm；
Flowing phase: methanol-acetonitrile-1mmol/L ammonium acetate solution, uses gradient elution；
Described gradient elution program is as follows: 0～1min, 85%～45%A, 10%B,
5%～45%C；1～2.5min, 45%A, 10%B, 45%C；2.5～7min,
45%～31%A, 10%～14%B, 45%C；7～12min, 31%～0%A,
14%～50%B, 50%C；12～15min, 0%～85%A, 50%～10%B,
50%～5%C；3min is balanced under 85%A, 10%B, 5%C.
Flow velocity: 1mL min-1；
Column temperature: 35 DEG C；
Sample size 1 μ L；
Mass Spectrometry Conditions:
Ion source: electric spray ion source；
Source injection electric cation 5 500V；Anion-4 500V；
Ion source temperature: 350 DEG C；
Whole process is passed through nitrogen.
In order to verify method provided by the present invention, use official method and improved method respectively
Measure Bergeninum and Fructus Mangifera Indicae in commercially available 3 different batches and producer's reducing fever relieving cough syrup sample
The content of glycosides, result see table.
Claims (2)
1. a liquid mass spectrum series connection measures chimonin and the side of Bergeninum in reducing fever relieving cough syrup
Method, it is characterised in that described detection method comprises the steps: successively
Precision measures this product 1ml, is placed in 10mL abstraction pool, with methanol to sample in temperature
Spend 60 DEG C, static extraction 3min, repeats to extract 2 times, by extracting solution first after having extracted
Alcohol is settled to 20mL, draws 1mL in centrifuge tube, whirlpool 2min, 15000r/min from
Heart 3min, takes supernatant and carries out chromatography；
Described chromatographic condition is as follows:
Chromatographic condition is as follows:
Chromatographic column: Kromasil-C18 post, 50mm × 4.6mm × 5mm；
Mobile phase methanol-acetonitrile-1mmol/L ammonium acetate solution, uses gradient elution；
Flow velocity: 1mL min-1；
Column temperature: 35 DEG C；
Sample size 1 μ L；
Mass Spectrometry Conditions:
Ion source: electric spray ion source；
Source injection electric cation 5 500V；Anion-4 500V；
Ion source temperature: 350 DEG C；
Whole process is passed through nitrogen.
A kind of liquid mass spectrum series connection the most according to claim 1 measures in reducing fever relieving cough syrup
Chimonin and the method for Bergeninum, it is characterised in that described gradient elution program is such as
Under: 0～1min, 85%～45%A, 10%B, 5%～45%C；1～2.5min,
45%A, 10%B, 45%C；2.5～7min, 45%～31%A, 10%～14%B,
45%C；7～12min, 31%～0%A, 14%～50%B, 50%C；12～
15min, 0%～85%A, 50%～10%B, 50%～5%C；85%A,
3min is balanced under 10%B, 5%C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610263368.6A CN105866285A (en) | 2016-04-26 | 2016-04-26 | Method for measuring mangiferin and bergenin in heat-clearing cough-relieving syrup in manner of liquid mass spectrum serial connection |
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|---|---|---|---|
| CN201610263368.6A CN105866285A (en) | 2016-04-26 | 2016-04-26 | Method for measuring mangiferin and bergenin in heat-clearing cough-relieving syrup in manner of liquid mass spectrum serial connection |
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| CN1954871A (en) * | 2005-10-27 | 2007-05-02 | 北京奇源益德药物研究所 | Yanhouqing preparation for treating throat disease and its preparation method and quality control method |
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| US20090269772A1 (en) * | 2008-04-29 | 2009-10-29 | Andrea Califano | Systems and methods for identifying combinations of compounds of therapeutic interest |
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| CN101028320A (en) * | 2006-12-05 | 2007-09-05 | 广州加德恩医药有限公司 | Vegetable medicinal composition with hypoglycemic and hypolipidemic functions and its making method |
| US20090269772A1 (en) * | 2008-04-29 | 2009-10-29 | Andrea Califano | Systems and methods for identifying combinations of compounds of therapeutic interest |
| US20110160152A1 (en) * | 2009-12-29 | 2011-06-30 | Taipei Medical University | Extracts of aquilaria hulls and use thereof in the treatment of cancer |
| CN101890071A (en) * | 2010-07-08 | 2010-11-24 | 上海中药标准化研究中心 | Method for identifying Gentiana rigescens Franch and Gentiana manshurica Kitag medicinal materials |
| EP2716637B1 (en) * | 2011-05-30 | 2017-07-19 | KPC Pharmaceuticals, Inc. | Mangiferin aglycone crystal form i and preparation method thereof |
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Application publication date: 20160817 |