CN105866284A - Method for simultaneously detecting three components in syrup capable of clearing away heat and relieving cough - Google Patents
Method for simultaneously detecting three components in syrup capable of clearing away heat and relieving cough Download PDFInfo
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- CN105866284A CN105866284A CN201610263367.1A CN201610263367A CN105866284A CN 105866284 A CN105866284 A CN 105866284A CN 201610263367 A CN201610263367 A CN 201610263367A CN 105866284 A CN105866284 A CN 105866284A
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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 simultaneously detecting three components in syrup capable of clearing away heat and relieving cough and aims at providing the method for simultaneously detecting the three components in the syrup capable of clearing away heat and relieving cough, which has good repeatability, high sensitivity and accurate result. The method comprises the following steps: precisely measuring 1ml of the product and putting the product into a 10-ml measuring flask; adding acetonitrile and diluting to a scale; shaking and taking supernatant; filtering with a 0.22-micron micro-pore filter membrane to obtain a solution of a test sample; and injecting 2 microliters of the solution of the test sample into a liquid chromatograph, wherein chromatographic conditions are as follows: a phase A of a mobile phase is methanol-water and a phase B of the mobile phase is acetonitrile-water-0.5% phosphoric acid water solution; the volume ratio of the methanol to the water in the phase A is 5 to 95; the volume ratio of the acetonitrile to the water to the 0.5% phosphoric acid water solution in the phase B is 10 to 70 to 10; the flow speed is 0.8mL/min and gradient elution is adopted; the detection wavelength is 226nm and 276nm; a detector is a PAD; and the column temperature is 35 DEG C. The method belongs to the technical field of chemical detection.
Description
Technical field
The invention provides a kind of method of three kinds of compositions in reducing fever relieving cough syrup of detection simultaneously；
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 favorable reproducibility, highly sensitive, result is same accurately
Time detection reducing fever relieving cough syrup in the method for three kinds of compositions.
For solving above-mentioned technical problem, the technical scheme that the present invention provides is as follows:
In a kind of reducing fever relieving cough syrup of detection simultaneously, the method for three kinds of compositions, includes following step successively
Rapid:
1) precision measures this product 1ml, puts in 10ml measuring bottle, adds dilution in acetonitrile to scale,
Shaking, takes supernatant, and 0.22 μm microporous filter membrane filters, and obtains need testing solution；
2) taking need testing solution 2 μ l and inject chromatograph of liquid, described chromatographic condition is such as
Under:
Mobile phase A is methanol-water mutually；B phase is acetonitrile-water-0.5% phosphate aqueous solution；Described
A phase in methanol and water volume ratio 5:95, acetonitrile, water, 0.5% phosphate aqueous solution in B phase
Volume ratio be 10:70:10；
Flow velocity is 0.8mL/min, uses gradient elution；
Detection wavelength is: 226nm, 276nm；
Detector: PAD；
Column temperature is 35 DEG C.
Further, the side of three kinds of compositions in above-mentioned a kind of reducing fever relieving cough syrup of detection simultaneously
Method, three kinds of described compositions refer to that Quercetin-3-O-β-D-Glucose-7-O-β-D-Radix Gentianae is double
Glucosides, praeruptorin A and chimonin.
Further, the side of three kinds of compositions in above-mentioned a kind of reducing fever relieving cough syrup of detection simultaneously
Method, gradient elution program: 0～2.5min, 20%A, 80%B；2.5-6min, 30%～
70%A, 70%～30%B；6-10min, 90%A, 10%B；Under 2%A, 98%B
Balance 3min.
Compared with prior art, the technical scheme that the present invention provides uses the side of gradient elution
Method, simultaneously Quercetin-3-O-β-D-Glucose-7-O-β-D-dragon in detection reducing fever relieving cough syrup
Gallbladder disaccharidase glycosides, praeruptorin A and chimonin, favorable reproducibility, highly sensitive, result is accurate
Truly have the quality beneficially controlling 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 method of three kinds of compositions in reducing fever relieving cough syrup of detection simultaneously, specifically, be
Quercetin-3-O-β-D-Glucose-7-O-β-D-gentiobiose in detection reducing fever relieving cough syrup
Glycosides, praeruptorin A and chimonin comprise the steps: successively
1) precision measures this product 1ml, puts in 10ml measuring bottle, adds dilution in acetonitrile to scale,
Shaking, takes supernatant, and 0.22 μm microporous filter membrane filters, and obtains need testing solution；
2) taking need testing solution 2 μ l and inject chromatograph of liquid, described chromatographic condition is such as
Under:
Mobile phase A is methanol-water mutually；B phase is acetonitrile-water-0.5% phosphate aqueous solution；Described
A phase in methanol and water volume ratio 5:95, acetonitrile, water, 0.5% phosphate aqueous solution in B phase
Volume ratio be 10:70:10；
Flow velocity is 0.8mL/min, uses gradient elution；
Detection wavelength is: 226nm, 276nm；
Detector: PAD；
Column temperature is 35 DEG C.
Gradient elution program: 0～2.5min, 20%A, 80%B；2.5-6min, 30%～
70%A, 70%～30%B；6-10min, 90%A, 10%B；Under 2%A, 98%B
Balance 3min.
In order to verify method provided by the present invention, use official method and improved method respectively
Measure Quercetin-3-O-β-D-in commercially available 3 different batches and producer's reducing fever relieving cough syrup sample
Glucose-7-O-β-D-gentiobioside with cape jasmine, praeruptorin A and chimonin content, result is shown in
Following table.
Claims (3)
1. detecting a method for three kinds of compositions in reducing fever relieving cough syrup, its feature exists simultaneously
In, comprise the steps: successively
1) precision measures this product 1ml, puts in 10ml measuring bottle, adds dilution in acetonitrile to scale,
Shaking, takes supernatant, and 0.22 μm microporous filter membrane filters, and obtains need testing solution；
2) taking need testing solution 2 μ l and inject chromatograph of liquid, described chromatographic condition is such as
Under:
Mobile phase A is methanol-water mutually；B phase is acetonitrile-water-0.5% phosphate aqueous solution；Described
A phase in methanol and water volume ratio 5:95, acetonitrile, water, 0.5% phosphate aqueous solution in B phase
Volume ratio be 10:70:10；
Flow velocity is 0.8mL/min, uses gradient elution；
Detection wavelength is: 226nm, 276nm；
Detector: PAD；
Column temperature is 35 DEG C.
One the most according to claim 1 detects three kinds of one-tenth in reducing fever relieving cough syrup simultaneously
The method divided, it is characterised in that three kinds of described compositions refer to Quercetin-3-O-β-D-Fructus Vitis viniferae
Sugar-7-O-β-D-gentiobioside with cape jasmine, praeruptorin A and chimonin.
One the most according to claim 1 detects three kinds of one-tenth in reducing fever relieving cough syrup simultaneously
The method divided, it is characterised in that gradient elution program: 0～2.5min, 20%A,
80%B；2.5-6min, 30%～70%A, 70%～30%B；6-10min, 90%A,
10%B；3min is balanced under 2%A, 98%B.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610263367.1A CN105866284A (en) | 2016-04-26 | 2016-04-26 | Method for simultaneously detecting three components in syrup capable of clearing away heat and relieving cough |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610263367.1A CN105866284A (en) | 2016-04-26 | 2016-04-26 | Method for simultaneously detecting three components in syrup capable of clearing away heat and relieving cough |
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| CN105866284A true CN105866284A (en) | 2016-08-17 |
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| CN201610263367.1A Pending CN105866284A (en) | 2016-04-26 | 2016-04-26 | Method for simultaneously detecting three components in syrup capable of clearing away heat and relieving cough |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103048409A (en) * | 2013-01-08 | 2013-04-17 | 广东台城制药股份有限公司 | Method for simultaneously detecting contents of four effective ingredients in antitussive tablet |
| CN104345110A (en) * | 2013-08-08 | 2015-02-11 | 河北以岭医药研究院有限公司 | Content determination method for seven compositions in traditional Chinese medicine composition preparation |
-
2016
- 2016-04-26 CN CN201610263367.1A patent/CN105866284A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103048409A (en) * | 2013-01-08 | 2013-04-17 | 广东台城制药股份有限公司 | Method for simultaneously detecting contents of four effective ingredients in antitussive tablet |
| CN104345110A (en) * | 2013-08-08 | 2015-02-11 | 河北以岭医药研究院有限公司 | Content determination method for seven compositions in traditional Chinese medicine composition preparation |
Non-Patent Citations (3)
| Title |
|---|
| 李红燕等: "HPLC测定除痰止嗽丸中的桔梗皂苷D、桔梗皂苷E、白花前胡甲素和白花前胡乙素", 《中国实验方剂学杂志》 * |
| 闫晓楠等: "HPLC法测定小儿咳宁糖浆中芒果苷的含量", 《齐鲁药事》 * |
| 黄丽玫等: "RP-HPLC法测定小儿清肺化痰口服液中槲皮素-3-O-β-D-葡萄糖-7-O-β-D-龙胆双糖苷的含量", 《中国药房》 * |
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Application publication date: 20160817 |