CN105974005A - Method for determining praeruptorin A in heat-clearing and cough-relieving syrup through liquid chromatography tandem mass spectrometry - Google Patents
Method for determining praeruptorin A in heat-clearing and cough-relieving syrup through liquid chromatography tandem mass spectrometry Download PDFInfo
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- CN105974005A CN105974005A CN201610263397.2A CN201610263397A CN105974005A CN 105974005 A CN105974005 A CN 105974005A CN 201610263397 A CN201610263397 A CN 201610263397A CN 105974005 A CN105974005 A CN 105974005A
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- praeruptorin
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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
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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 invention provides a method for determining multiple components in heat-clearing and cough-relieving syrup through liquid chromatography tandem mass spectrometry, and aims to provide the simple method for determining the multiple components in the heat-clearing and cough-relieving syrup through the liquid chromatography tandem mass spectrometry, wherein the method has good chromatographic peak separation degree The method comprises the steps: precisely measuring to take 1 mL a of the syrup, placing the syrup in a 10 mL extraction tank, making the volume of the sample to be constant at 20 mL in methanol with methanol, sucking 1 mL to a centrifuge tube, whirling for 2 min, centrifuging for 3 min at the rotation speed of 15000 r/min, taking a supernatant, and carrying out 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 process and measure Peucedanum praeruptorum DUNN in reducing fever relieving cough syrup
The method of A prime；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 liquid mass spectrum a kind of simple to operate, that chromatographic peak separating degree is good
Series process measures the method for Multiple components in reducing fever relieving cough syrup.
A kind of liquid mass spectrum series process measures the method for praeruptorin A in reducing fever relieving cough syrup,
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 80 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: Diamonsil C 18,
Flowing is methanol A mutually, 0.1% aqueous formic acid B, uses gradient elution；
Flow velocity is 1mL min-1；
Column temperature 30 DEG C；
Sample size 5 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 mass spectrum series process measures before spending in vain in reducing fever relieving cough syrup
The method of Hu Jiasu, described chromatographic column specification: 4.6mm × 150mm, 5 μm.
Further, above-mentioned a kind of mass spectrum series process measures before spending in vain in reducing fever relieving cough syrup
The method of Hu Jiasu, described gradient elution program is as follows: 0～2.5min, 5%～
55%A, 95%～5%B；2.5～5.5min, 55%～95%A, 5%～45%B；
5.5～12min, 98%A, 2%B.
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 in detection reducing fever relieving cough syrup, the method
Simple to operate, favorable reproducibility, high-specificity, chromatographic peak separating degree is good, is conducive to controlling to produce
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
A kind of liquid mass spectrum series process measures the method for praeruptorin A in reducing fever relieving cough syrup,
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 80 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: Diamonsil C 18 (4.6mm × 150mm, 5 μm),
Flowing is methanol A mutually, 0.1% aqueous formic acid B, uses gradient elution；
Described gradient elution program is as follows: 0～2.5min, 5%～55%A, 95%～
5%B；2.5～5.5min, 55%～95%A, 5%～45%B；5.5～12min,
98%A, 2%B.
Flow velocity is 1mL min-1；
Column temperature 30 DEG C；
Sample size 5 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 praeruptorin A in commercially available 3 different batches and producer's reducing fever relieving cough syrup sample
Content, result see table.
Claims (3)
1. a liquid mass spectrum series process measures the side of praeruptorin A 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 80 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: Diamonsil C 18,
Flowing is methanol A mutually, 0.1% aqueous formic acid B, uses gradient elution；
Flow velocity is 1mL min-1；
Column temperature 30 DEG C；
Sample size 5 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 mass spectrum series process the most according to claim 1 measures in reducing fever relieving cough syrup
The method of praeruptorin A, it is characterised in that described chromatographic column specification: 4.6mm ×
150mm, 5 μm.
A kind of mass spectrum series process the most according to claim 1 measures in reducing fever relieving cough syrup
The method of praeruptorin A, it is characterised in that described gradient elution program is as follows:
0～2.5min, 5%～55%A, 95%～5%B；2.5～5.5min, 55%～
95%A, 5%～45%B；5.5～12min, 98%A, 2%B.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610263397.2A CN105974005A (en) | 2016-04-26 | 2016-04-26 | Method for determining praeruptorin A in heat-clearing and cough-relieving syrup through liquid chromatography tandem mass spectrometry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610263397.2A CN105974005A (en) | 2016-04-26 | 2016-04-26 | Method for determining praeruptorin A in heat-clearing and cough-relieving syrup through liquid chromatography tandem mass spectrometry |
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| Publication Number | Publication Date |
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| CN105974005A true CN105974005A (en) | 2016-09-28 |
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|---|---|---|---|
| CN201610263397.2A Pending CN105974005A (en) | 2016-04-26 | 2016-04-26 | Method for determining praeruptorin A in heat-clearing and cough-relieving syrup through liquid chromatography tandem mass spectrometry |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103006725A (en) * | 2013-01-09 | 2013-04-03 | 徐国兵 | Medical composition for treating diabetes mellitus with hyperlipaemia and preparation method thereof |
| CN103048409B (en) * | 2013-01-08 | 2014-01-01 | 广东台城制药股份有限公司 | Method for simultaneously detecting contents of four effective ingredients in antitussive tablet |
| CN104569252A (en) * | 2014-12-15 | 2015-04-29 | 广州白云山陈李济药厂有限公司 | Establishment method of fingerprint spectrum of traditional Chinese medicine composition |
| CN105334286A (en) * | 2015-11-25 | 2016-02-17 | 吉林修正药业新药开发有限公司 | Quality control method for medicine for treating common cold due to wind-cold |
-
2016
- 2016-04-26 CN CN201610263397.2A patent/CN105974005A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103048409B (en) * | 2013-01-08 | 2014-01-01 | 广东台城制药股份有限公司 | Method for simultaneously detecting contents of four effective ingredients in antitussive tablet |
| CN103006725A (en) * | 2013-01-09 | 2013-04-03 | 徐国兵 | Medical composition for treating diabetes mellitus with hyperlipaemia and preparation method thereof |
| CN104569252A (en) * | 2014-12-15 | 2015-04-29 | 广州白云山陈李济药厂有限公司 | Establishment method of fingerprint spectrum of traditional Chinese medicine composition |
| CN105334286A (en) * | 2015-11-25 | 2016-02-17 | 吉林修正药业新药开发有限公司 | Quality control method for medicine for treating common cold due to wind-cold |
Non-Patent Citations (2)
| Title |
|---|
| 王秀敏 等: "液相色谱-串联质谱法研究白花前胡甲素脂质体在大鼠体内的药动学", 《中国新药与临床杂志》 * |
| 陈存武 等: "LC-MS分析早薹对白花前胡根化学成分的影响", 《食品与生物技术学报》 * |
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Application publication date: 20160928 |
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