Content detection method for compound houttuynia cordata mixture

A compound Houttuynia cordata and detection method technology, which is applied in the fields of pharmacy and analytical chemistry, can solve the problems of quercitrin and baicalin loss and non-detection, and achieve the effects of ensuring clinical efficacy, simple operation, and eliminating carbohydrate interference

Active Publication Date: 2015-08-05
浙江康恩贝中药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This is because the composition of the compound Houttuynia mixture contains not only forsythin, but also flavonoid glycosides such as baicalin and quercitrin, but neutral alumina will combine with the ortho-diphenolic hydroxyl group in flavonoids, "3 -Hydroxy, 4-keto", "5-hydroxyl, 4-keto" complexation produces dead adsorption, resulting in serious loss of quercitrin and baicalin, and these two components are basically undetectable

Method used

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  • Content detection method for compound houttuynia cordata mixture
  • Content detection method for compound houttuynia cordata mixture
  • Content detection method for compound houttuynia cordata mixture

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Embodiment 1, chromatographic column investigation

[0059] Column type:

[0060] 1#: Agilent ZORBAX SB-C18, the column length is 250mm, the inner diameter is 4.6mm, and the packing particle size is 5μm;

[0061] 2#: Agilent ZORBAX Eclipse XDB-C18, the column length is 250mm, the inner diameter is 4.6mm, and the packing particle size is 5μm;

[0062] 3#: Agilent ZORBAX SB-Phenyl, the column length is 250mm, the inner diameter is 4.6mm, and the packing particle size is 5μm;

[0063] A, preparation of reference substance solution:

[0064] Take quercetin, baicalin, and forsythin reference substances respectively, use methanol as solvent, dilute and prepare a mixed standard solution, and prepare a concentration of 0.016mg / ml quercetin, 0.45mg / ml baicalin, 0.020mg / ml ml forsythin reference substance solution;

[0065] B. Preparation of the test solution:

[0066] Precisely draw 25.0ml of the test product, and shake it for 3 times with water-saturated n-butanol, 25ml ea...

Embodiment 2

[0070] Embodiment 2, chromatographic condition investigation

[0071] The preparation method of reference substance solution and need testing solution is with embodiment 1, and detection condition is as follows:

[0072] Chromatographic condition 1: Refer to "Simultaneous Determination of Chlorogenic Acid, Forsythin and Baicalin in Compound Houttuynia Tablets by RP-HPLC", with octadecylsilane bonded silica gel as filler and acetonitrile as mobile phase A , 0.002% phosphoric acid solution was the mobile phase B, and carried out gradient elution according to the elution conditions in Table 1; the flow rate was 1.0ml / min and the detection wavelength was 280nm; 10 μL of the reference substance solution and the test solution were injected into the liquid chromatograph for determination , that is. see attached results Figure 4 .

[0073] Table 1 Elution conditions

[0074] time (min)

Mobile phase A(%)

Mobile phase B(%)

0

10

90

6

30

...

Embodiment 3

[0078] Embodiment 3, need testing solution preparation method-extraction solvent, consumption, frequency investigation

[0079] A, preparation of reference substance solution:

[0080] Take quercetin, baicalin, and forsythin reference substances respectively, use methanol as solvent, dilute and prepare a mixed standard solution, and prepare a concentration of 0.016mg / ml quercetin, 0.45mg / ml baicalin, 0.020mg / ml ml forsythin reference substance solution;

[0081] B. Preparation of the test solution:

[0082] Precisely draw 25.0ml of compound Houttuynia cordata mixture (batch number: 130708), nine copies, and carry out the test: design the extraction solvent, solvent dosage and extraction times according to the L9(34) orthogonal table, and perform orthogonal according to Table 2, see the orthogonal results Table 3 to Table 6. Combine the extracts, evaporate to dryness, add 10ml of water to the residue to dissolve, pass through a D101 macroporous resin column (inner diameter 1...

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Abstract

The invention discloses a content detection method for a compound houttuynia cordata mixture. The content detection method mainly includes that water-saturated normal butanol is used for extraction, water-alcohol elution is performed after column feeding, Phenyl bonded silica gel is taken as a chromatographic column, and mobile phase is acetonitrile-0.5% acetic acid solution (volume ratio is 18.5:81.5). By the content detection method, the problem that quercitrin which serves as a feature ingredient of the compound houttuynia cordata mixture cannot be controlled effectively is solved, content of quercitrin, baicalin and forsythin in the compound houttuynia cordata mixture is detected synchronously, and drug safety, effectiveness and quality controllability are guaranteed.

Description

technical field [0001] The invention belongs to the technical field of pharmacy and analytical chemistry, and in particular relates to a content detection method of compound houttuynia mixture. Background technique [0002] Compound Houttuynia Herba Mixture has the effect of clearing heat and detoxifying. For sore throat caused by exogenous wind-heat; acute pharyngitis, tonsillitis with wind-heat syndrome. [0003] [0004] Preparation method: decoct the above five medicinal materials with water twice, 2 hours each time, combine the decoction liquid, filter, concentrate the filtrate to a clear paste with a relative density of 1.18-1.20 (60°C-80°C), add ethanol to precipitate Stir until the alcohol content is 70%, let it stand for 24 hours, filter, and recover ethanol from the filtrate under reduced pressure and concentrate to an appropriate amount. Take another 60g of sucrose to make a simple syrup, add the above liquid medicine, add the prescribed amount of honey, sodi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/08
Inventor 王如伟金汉台印晓红王建方吴健何厚洪陈卿兰文一
Owner 浙江康恩贝中药有限公司
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