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HPLC (High Performance Liquid Chromatography) fingerprint spectrum of tablet capable of promoting blood circulation and eliminating goiter, and preparation method thereof

A fingerprint and Xiaoying tablet technology is applied in the field of fingerprint detection of Huoxue Xiaoying tablets, and achieves the effects of high method precision, convenient operation and good peak shape.

Active Publication Date: 2019-09-17
WUHAN AIMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chromatography mainly includes thin-layer chromatography, high-performance liquid chromatography, gas chromatography, etc. Among them, high-performance liquid chromatography (HPLC) has the characteristics of high efficiency, rapidity, sensitivity and good reproducibility, and has now become the mainstream method for the study of fingerprints of traditional Chinese medicine. , but there is no report that this method is used for the quality control of Huoxue Xiaoying Tablets

Method used

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  • HPLC (High Performance Liquid Chromatography) fingerprint spectrum of tablet capable of promoting blood circulation and eliminating goiter, and preparation method thereof
  • HPLC (High Performance Liquid Chromatography) fingerprint spectrum of tablet capable of promoting blood circulation and eliminating goiter, and preparation method thereof
  • HPLC (High Performance Liquid Chromatography) fingerprint spectrum of tablet capable of promoting blood circulation and eliminating goiter, and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1. Sample pretreatment

[0045] Preparation of the test solution: Huoxue Xiaoying Tablets (0.6g / tablet), take 10 tablets, grind into fine powder, accurately weigh about 2.000g, place in a 100ml volumetric flask, and accurately add ethanol with a volume concentration of 70%. 50ml of aqueous solution, weighed, sealed with an ultrasonic instrument for 30min, then weighed again, supplemented the lost weight with 70% ethanol, centrifuged at 3000r / min for 20min, took the supernatant, and used a pore size of 0.22μm filter membrane to obtain the test solution.

[0046] Preparation of mixed reference substance solution: Accurately weigh erine, amygdalin, wangbulixing flavonoid glycoside, saikosaponin B2, saikosaponin B1, bisdemethoxycurcumin, demethoxycurcumin and gemacerone reference substance, placed in a volumetric flask for gradual dilution, that is, adding 70% ethanol aqueous solution to dissolve and shake up at a constant volume in a volumetric flask to obtain a reference...

Embodiment 2

[0073] The optimization of embodiment 2 chromatographic conditions

[0074] 1. Selection of wavelength

[0075] Wavelength: 230nm, 250nm, 280nm

[0076] Select different detection wavelengths and perform elution according to the gradient program in Table 5. The gradient elution program in Table 5 was adopted before the elution program in Table 2 was determined. The fingerprints of the three wavelengths are shown in Figure 4 .

[0077] table 5

[0078] time / min Mobile phase A / % (volume) Mobile phase B / % (volume) 0～15 0 100 15～20 11 89 20～35 11→24 89→76 35～40 24→54 76→46 40～50 54→90 46→10 50～61 90→0 10→100 61～70 0 100

[0079] It can be seen that compared with 230nm and 280nm, the number of chromatographic peaks with a detection wavelength of 250nm is significantly increased, and the peak height is significantly enhanced, especially at 60-70min, the number of peaks at 280nm is significantly less than 250nm. The chr...

Embodiment 3

[0086] The detection of embodiment 3 samples

[0087] Three batches of samples were re-prepared, and their fingerprints were tested under the above conditions respectively. The comparison results of the similarity between each batch and the generated standard spectrum are shown in Table 6, which shows that the method has good reproducibility, and each batch is similar to the reference standard spectrum. The degree is greater than 0.9, which is suitable for the detection of the characteristic fingerprint of Huoxue Xiaoying Tablets.

[0088] Table 6 Similarity Calculation Results

[0089] sample S1 190404 190406 190407 Control Fingerprint S1 1 0.909 0.916 0.904 0.934 190404 0.909 1 0.932 0.937 0.978 190406 0.916 0.932 1 0.954 0.974 190407 0.904 0.937 0.954 1 0.977 Control Fingerprint 0.934 0.978 0.974 0.977 1

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Abstract

The invention discloses a HPLC (High Performance Liquid Chromatography) fingerprint spectrum of a tablet capable of promoting blood circulation and eliminating a goiter. The method for preparing the fingerprint spectrum comprises the following steps that: independently detecting the solution of a sample for testing, hybrid reference substance solution, singe medicine material sample solution and sample-lacking negative sample solution on a high performance liquid chromatograph, wherein the high performance liquid chromatograph contains an ultraviolet detector, the set detection wavelength of the ultraviolet detector is 240-260nm, the stationary phase of the high performance liquid chromatograph is a C18 bonded silica gel chromatographic column, a mobile phase A is acetonitrile, and a mobile phase B is 0.05-0.2% trifluoroacetic acid aqueous solution; and adopting gradient elution. The spectrum contains 15 pieces of common fingerprint peaks, the fingerprint spectrum can be used for carrying out affiliation positioning and content measurement on eight index components and five traditional Chinese medicine ingredients in the tablet capable of promoting a blood circulation and eliminating the goiter, so that the comprehensive detection of the chemical ingredients of the tablet capable of promoting a blood circulation and eliminating the goiter can be realized, and the internal quality of the traditional Chinese medicines can be more comprehensively reflected and controlled.

Description

technical field [0001] The invention belongs to the field of detection of traditional Chinese medicines, and relates to a method for detecting fingerprints of Huoxuexiaoying Tablets and an application thereof. Background technique [0002] CN104173922A discloses a traditional Chinese medicine, which is made of peach kernel, curcuma, bupleurum, cat's claw grass, buliuxing, dung beetle, soil beetle, and centipede eight flavors of Chinese medicinal materials. Knot-based, supplemented by heat-clearing and detoxifying, soothing the liver and relieving stagnation, it has a good effect on the treatment of galls, and the trade name is Huoxuexiaoying Tablets. [0003] At present, the quality control of Huoxue Xiaoying Tablets is mainly realized through the content determination and TLC identification of one or two index components. However, the curative effect of traditional Chinese medicine is produced through the comprehensive action of multiple components and multiple targets. Th...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/8809
Inventor 叶利春石召华肖静霞梁云柳畅胡俊杰曾晓玲郑娇娇
Owner WUHAN AIMIN PHARMA
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