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Fingerprint spectrum of xiaocaihu compound preparation, construction method of fingerprint spectrum and content determination method of xiaocaihu compound preparation

A technology for compound preparations and construction methods, which can be applied to measurement devices, instruments, scientific instruments, etc., can solve the problems of poor resolution, few common peaks in fingerprints, long time consumption, etc., and achieve effective quality detection and no peak shape. Interference, good peak shape effect

Active Publication Date: 2021-07-20
CHINA RESOURCES SANJIU MEDICAL & PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Therefore, the purpose of the present invention is to solve the common peak number of the fingerprint chromatogram obtained by the construction method of the xiaobupleurum compound preparation fingerprint chromatogram in the prior art, and the resolution is not high. In view of the problems of good quality and long time consumption, a fingerprint of Xiaobupleurum compound preparation and its construction method are provided

Method used

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  • Fingerprint spectrum of xiaocaihu compound preparation, construction method of fingerprint spectrum and content determination method of xiaocaihu compound preparation
  • Fingerprint spectrum of xiaocaihu compound preparation, construction method of fingerprint spectrum and content determination method of xiaocaihu compound preparation
  • Fingerprint spectrum of xiaocaihu compound preparation, construction method of fingerprint spectrum and content determination method of xiaocaihu compound preparation

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0068] The investigation of experimental example 1 extraction solvent

[0069] 1. Instruments and reagents:

[0070] Nexera X2 series Shimadzu LC-30A ultra-high performance liquid chromatograph, METTLER TOLEDO electronic balance PL402-L, METTLER TOLEDO XS 105 analytical balance, FA1004 electronic balance (Shanghai Yueping Scientific Instrument Co., Ltd.), KQ-300B ultrasonic cleaner (Kunshan Ultrasonic Instrument Co., Ltd.), H / T16M desktop high-speed centrifuge (Hunan Hexi Instrument Equipment Co., Ltd.). The water used for chromatographic analysis was pure drinking water from Wahaha, the methanol and acetonitrile were chromatographically pure (Fisher), and the formic acid was analytically pure; the methanol and ethanol used for extraction were both analytically pure. See Table 1 for information on the standards used in the experiments.

[0071] Table 1 Standard product information

[0072]

[0073] 2. Experimental method:

[0074] (1) Preparation of test solution

[00...

experiment example 2

[0088] Determination of Experimental Example 2 Chromatographic Conditions

[0089] 1. Selection of detection wavelength

[0090] In the initial stage of the present invention, four wavelengths of 210nm, 254nm, 270nm, and 330nm have been investigated. The experimental results show that the components of Bupleuri are completely characterized at 254nm (retention time 21-23min), and the response values ​​at other wavelengths are too low. Therefore, the optimum wavelength is 254nm (See image 3 and Figure 4 ).

[0091] 2. Selection of mobile phase and optimization of gradient conditions

[0092] Except the gradient program and mobile phase, all the other chromatographic conditions are the same as in Example 1, with the gradient program and mobile phase as variables, a plurality of different elution gradients and mobile phases (gradient conditions 1-2 and optimized gradient conditions 3 -11, see table 3-7) measure the same part of need testing solution, the results are shown in...

experiment example 3

[0111] The selection of experimental example 3 reference substance

[0112] 1. Experimental method

[0113] Preparation of reference substance solution: Accurately weigh saikosaponin a reference substance and saikosaponin d reference substance, add methanol to dissolve, and constant volume to prepare reference substance solutions with concentrations of 241.33 μg / ml and 65.33 μg / ml respectively.

[0114] Ultra-high performance liquid phase test: the above-mentioned need testing solution and reference substance solution are respectively injected in the Shimadzu LC-30A ultra-high performance liquid chromatograph for detection, and the injection volume is 3 μ l, respectively with acetonitrile (A)-water (B ) and acetonitrile (A)-0.5% formic acid aqueous solution (B) as the mobile phase for detection, gradient elution, the elution conditions are as follows, 0~2min, 17%A; 2~4min, 17~20%A; 4~7.5 min, 20~28%A; 7.5~10min, 28%A; 10.5~16min, 28~35%; 16~18min, 35~50%A; 18~21min, 50~52%A; ...

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Abstract

The invention belongs to the technical field of quality detection of traditional Chinese medicine preparations, and particularly provides a fingerprint spectruma of a xiaocaihu compound preparation, a construction method of the fingerprint spectrum and a content determination method of the xiaocaihu compound preparation, and the construction method of the xiaocaihu compound preparation fingerprint spectrum comprises the following steps: (1) preparing a xiaocaihu compound preparation test solution; and (2) taking a test solution of the xiaocaihu compound preparation, performing detecting by adopting a high performance liquid chromatography, carrying out gradient elution by taking octadecylsilane chemically bonded silica as a filler and formic acid aqueous solution-acetonitrile as a mobile phase, and carrying out repeated tests to obtain an elution procedure. Under the elution condition, the number of common peaks is obviously increased, the separation degree of common characteristic peaks is obviously improved, the detection time is greatly shortened, and the common peaks are good in peak shape and free of interference, so that the quality of the Under the elution condition, the number of common peaks is obviously increased;xiaocaihu compound preparation can be detected more comprehensively, clearly and effectively.

Description

technical field [0001] The invention belongs to the technical field of quality detection of traditional Chinese medicine preparations, and in particular relates to a fingerprint of a compound preparation of Xiaobupleurum and its construction method, and a method for determining the content of a compound preparation of Xiaobupleuri. Background technique [0002] Xiaochaihu granule is a compound preparation obtained by mixing, concentrating, and granulating the aqueous extracts of Bupleurum, Scutellaria, Codonopsis, and Jujube with ginger pinellia and 70% ethanol extracts of ginger. It is used to treat diseases caused by exogenous pathogenic factors, evil offender Shaoyang syndrome, symptoms include alternating cold and heat, bitter fullness in the chest and hypochondrium, loss of appetite, restlessness and vomiting, bitter mouth and dry throat. [0003] The State Food and Drug Administration has a total of 98 companies with production batch numbers for Xiaochaihu granules. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 张雪刘晖晖吴宏伟杨洪军林丽娜马鹏岗
Owner CHINA RESOURCES SANJIU MEDICAL & PHARMA
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