Method for simultaneously determining four effective components in Gongying Qinglan granules

A technology of active ingredients and determination methods, which is applied in the field of simultaneous determination of four active ingredients in Gongying Qinglan Granules, can solve the problems of inability to detect active ingredients at the same time, complicated preparation of thin-layer chromatography, and difficult identification of thin-layer spots, and achieve chromatographic peaks The effect of good peak shape, good reproducibility of results, and moderate peak area response

Pending Publication Date: 2021-10-12
魏秀丽 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Among the above standard methods, the three TLC identifications are caffeic acid, baicalin and berberine hydrochloride respectively. The pretreatment methods are different, and the solvents used are various and highly toxic: benzene-ethyl acetate-methanol-isopropanol- Concentrated ammonia test solution-butanone-n-butanol formic acid-glacial acetic acid, etc., are more harmful to experimenters
In addition, the pre-preparation of thin-layer chromatography in this scheme is complicated, and some require multiple steps such as pre-saturation, unfolding, drying, spraying, checking and checking the results, etc., which is time-consuming and labor-intensive, and is greatly affected by factors such as environmental temperature and humidity, and edge effects, etc. , thin-layer spots are sometimes difficult to distinguish, and the reproducibility is poor; therefore, thin-layer identification of spots is greatly affected by environmental temperature, humidity and human operation.
[0014] In the standard, only one component of chlorogenic acid is determined, and other active components cannot be detected at the same time

Method used

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  • Method for simultaneously determining four effective components in Gongying Qinglan granules
  • Method for simultaneously determining four effective components in Gongying Qinglan granules
  • Method for simultaneously determining four effective components in Gongying Qinglan granules

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0084] Simultaneous determination method of 4 active ingredients in Gongying Qinglan Granules. The 4 active ingredients are chlorogenic acid, caffeic acid, berberine hydrochloride, and baicalin. The assay method includes the following steps:

[0085] a. Preparation of standard stock solution and mixed standard stock solution

[0086] Take standard products of chlorogenic acid, caffeic acid, baicalin, and berberine hydrochloride, dissolve them in methanol and make up to volume, and prepare chlorogenic acid standard stock solution, caffeic acid standard stock solution, baicalin standard stock solution, and berberine hydrochloride Alkali standard stock solution; each standard stock solution is mixed to obtain a mixed standard stock solution, see Table 3 below for details:

[0087] table 3

[0088]

[0089] b. Preparation of sample solution to be tested: Accurately weigh 1.0g of Gongyingqinglan granules for testing, place in a 25mL volumetric flask, dissolve with 70% ethanol a...

Embodiment 2

[0110] Simultaneous determination of 4 active ingredients in the Gongyingqinglan granule described in Example 1, the difference is:

[0111] In step b, prepare the sample solution to be tested: Accurately weigh 2.0 g of Gongyingqinglan granules as the test product, place it in a 50 mL volumetric flask, dissolve it with 70% ethanol and set the volume to the mark, extract 10 ml from it by ultrasonic extraction for 30 min, 10000 rpm / min centrifugal 5min, filter, and the filtrate is determined by liquid chromatography; other conditions and steps are the same as in Example 1.

experiment example

[0113] 1. The influence of different solvent treatment methods on the test results

[0114] Compare the impact of different solvent treatment methods on the test results. In step b, the sample solution to be tested is prepared from method A, method B or method C in table 5, method D, method E, method F, method G, method H, method , Method I, Method J.

[0115] table 5

[0116] serial number method Different Solvent Treatment Methods 1 Method A 70% ethanol:hydrochloric acid=100:0.5 2 Method B water 3 Method C 50% methanol 4 Method D (100 methanol: 1 hydrochloric acid): water = 1:1 5 Method E 5% methanol 6 Method F 50% ethanol 7 Method G (100 methanol: 5 hydrochloric acid): water = 1:1 8 Method H Absolute ethanol 9 Method I Methanol 10 Method J Methanol: hydrochloric acid = 100:1 11 Method K 70% ethanol

[0117] specific:

[0118] Method A is: accurately weigh 1.0 g of the...

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Abstract

The invention relates to a method for simultaneously determining four effective components in Gongying Qinglan granules. The method comprises the following steps: extracting a test sample by using 70% ethanol as an extraction solvent, and simultaneously determining the four main components at one time by using liquid chromatography. According to the invention, 278 nm, 324 nm and 346 nm are adopted as the wavelengths of the effective components, so baseline fluctuation is small, the response values of chlorogenic acid and caffeic acid are higher, and the response value of berberine hydrochloride is also taken into consideration; the method can be used for simultaneously determining the contents of chlorogenic acid, caffeic acid, baicalin and berberine hydrochloride in the Gongying Qinglan granules, and is rapid, sensitive, accurate and high in specificity; and the method can simultaneously determine the contents of the four components through one-time sample treatment, so not only is the reagent and time saved, but also working efficiency is improved.

Description

technical field [0001] The invention relates to a simultaneous determination method for four active components in Gongyingqinglan granules, belonging to the field of detection of active components in veterinary medicines. Background technique [0002] Gongying Qinglan Granules is a traditional Chinese veterinary medicine preparation, which is recorded in "Veterinary Drug Quality Standards" 2017 Edition (Chinese Medicine Volume) p97-98. The prescription is: Dandelion 200g, Folium Isatidis 200g, Radix Isatidis 200g, Honeysuckle 100g, Scutellaria baicalensis 100g, Phellodendron Phellodendri 100g, licorice 100g, Huoxiang 50g, gypsum 50g; the above 9 flavors, add water and decoct twice, combine the decoction, filter, and concentrate the filtrate to a clear paste with a relative density of 1.28-1.30. Take 1 part of the clear paste, add 1.6 parts of dextrin and 1 part of sucrose to make granules, dry, granulate, and make 900g. It is yellow-brown granules; bitter and slightly sweet....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/54G01N30/74
CPCG01N30/02G01N30/06G01N30/54G01N30/74
Inventor 魏秀丽张传津张志民王尚明陆庆泉汪安国魏茂莲
Owner 魏秀丽
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