Method for detecting contents of baicalin, forsythin, indirubin and glycyrrhizic acid in Qingreling granules

A technology of baicalin and Qingreling, which is applied in the field of content determination of traditional Chinese medicine preparations, can solve problems such as difficult to reflect the quality of medicines, and achieve the effects of saving time and testing costs, improving quality control standards, and controlling quality

Active Publication Date: 2014-04-02
CHIATAI QINGCHUNBAO PHARMA
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AI Technical Summary

Problems solved by technology

[0003] Qingreling granules only measure the content of baicalin in Scutellaria baicalensis under the content determination item in the "Pharmacopoeia of the People's Republic of China" 2010 edition, which is difficult to reflect the quality of the entire drug, and has certain deficiencies

Method used

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  • Method for detecting contents of baicalin, forsythin, indirubin and glycyrrhizic acid in Qingreling granules
  • Method for detecting contents of baicalin, forsythin, indirubin and glycyrrhizic acid in Qingreling granules
  • Method for detecting contents of baicalin, forsythin, indirubin and glycyrrhizic acid in Qingreling granules

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Experimental program
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Effect test

Embodiment 1

[0060] Example 1: The content of baicalin, forsythin, indirubin and glycyrrhizic acid in Qingreling granules was determined by high performance liquid chromatography.

[0061] (1) HPLC conditions

[0062] Instrument name: Agilent 1100 high performance liquid chromatograph

[0063] Chromatographic conditions: Column: ZORBAX SB-phenyl (column length 250mm, inner diameter 4.6mm), filler: phenyl-bonded silica gel (particle size 5μm), flow rate: 1.0ml / min, column temperature: 25°C

[0064] DAD UV detector detection wavelength: 280nm, 277nm, 289nm, 252nm

[0065] Use 0.5% glacial acetic acid aqueous solution as mobile phase A and acetonitrile as mobile phase B, and perform gradient elution according to Table 1.

[0066] Table 1 Gradient elution conditions

[0067] time (minutes)

Mobile phase A (%)

Mobile phase B (%)

0～20

80→72

20→28

20～35

72→57

28→43

35～50

57

43

[0068] (2) Preparation of standard solution:

...

Embodiment 2

[0086] Precisely weigh the baicalin standard, add 70% ethanol aqueous solution by volume, and prepare a standard solution containing 36 μg of baicalin per 1 ml.

[0087] Precisely weigh the standard substance of forsythin, add 70% ethanol aqueous solution by volume, and prepare a standard solution containing 100 μg of forsythin per 1 ml.

[0088] Precisely weigh the indirubin standard substance, add 70% ethanol aqueous solution by volume, and prepare a standard solution containing 2.8 μg of indirubin per 1 ml.

[0089] Accurately weigh the ammonium glycyrrhizinate standard, add 70% ethanol aqueous solution by volume to prepare a standard solution containing 120 μg of ammonium glycyrrhizinate per 1ml. (weight of glycyrrhizic acid = weight of ammonium glycyrrhizinate / 1.0207).

[0090] The volume concentration 50% ethanol aqueous solution in the step (3) in Example 1 was replaced with a volume concentration 70% ethanol aqueous solution, and the ultrasonic time was replaced from ...

Embodiment 3

[0092] The 50% ethanol aqueous solution of volume concentration in the preparation of the sample to be tested in Example 1 was replaced with the solution shown in Table 2, and the sample to be tested A was detected. Peak, record the peak area, the results are shown in Table 2.

[0093] It can be seen from Table 2 that the ethanol aqueous solution used in the preparation of the sample solution to be tested is preferably a 50% ethanol solution or a 70% ethanol solution. The reason is that baicalin, forsythin, baicalin, forsythin, The chromatographic peak areas of indirubin and glycyrrhizic acid were the largest when extracted with 50% ethanol solution and 70% ethanol solution.

[0094] Table 2 Influence of solvent on absorption peak

[0095]

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Abstract

The invention discloses a method for detecting contents of baicalin, forsythin, indirubin and glycyrrhizic acid in Qingreling granules. The method comprises the following steps: pretreating the Qingreling granules to prepare a sample to be detected, and injecting the sample to be detected to a high performance liquid chromatograph for detecting to obtain a high performance liquid chromatogram of the sample to be detected; and calculating the contents of the baicalin, the forsythin, the indirubin and the glycyrrhizic acid in the sample to be detected according to the peak areas of corresponding absorption peaks in the high performance liquid chromatogram of the sample to be detected and a standard curve of each standard sample. The method disclosed by the invention can be used for measuring the components of the baicalin under the content determination items of the Qingreling granules in the first part of Pharmacopoeia of the People's Republic of China published in 2010, and also can be used for additionally measuring the content of the forsythin in fructus forsythiae, the content of the indirubin in folium isatidis and the content of the glycyrrhizic acid in liquorice and greatly improving the quality control standard of the Qingreling granules. Proved through content measurement methodology, the method completely conforms to the specification and is an advanced quality control method. The method can be used for shortening the detection time and reducing the detection cost.

Description

(1) Technical field [0001] The invention relates to a method for determining the content of a traditional Chinese medicine preparation, in particular to a method for detecting the contents of baicalin, forsythin, indirubin and glycyrrhizic acid in Qingreling granules. (2) Background technology [0002] The prescription composition of Qingreling Granules is 250g of Scutellaria, 250g of Forsythia, 250g of Daqingye, and 50g of Licorice. The above four herbs are boiled twice with water for 1.5 hours each time, the filtrate is combined, filtered, the filtrate is concentrated to a clear paste with a relative density of 1.20-1.25 (80°C), cooled, and ethanol is added to make the alcohol content reach 58%~60%, let stand for more than 12 hours, filter the supernatant, recover ethanol from the filtrate and concentrate it to a thick paste with a relative density of 1.29~1.31 (80℃), add 740g of sucrose powder and an appropriate amount of dextrin to make granules , dried to make 1000g; o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 林徐剑吴碧元柴建国施晓萍沈莹
Owner CHIATAI QINGCHUNBAO PHARMA
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