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Xiaojin pill fingerprint detection method

A detection method and fingerprint technology, which is applied in the detection field of Xiaojin Pill fingerprints, can solve problems such as control, complex composition of medicinal flavors, and difficult overall quality of Xiaojin Pills, so as to achieve overall control, improve the quality evaluation system, and ensure the effect of clinical curative effect

Inactive Publication Date: 2020-01-07
CHENGDU UNIV OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The composition of Xiaojin Pills is complex, covering a large number of fat-soluble components and water-soluble components. The properties and polarities of various chemical components vary greatly. It is difficult for a conventional single fingerprint to reflect its whole picture, and it is difficult to carry out overall quality control on Xiaojin Pills.
At present, there is no research report on the fingerprint of Xiaojinwan

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1 Fingerprint detection of fat-soluble parts of Xiaojin Pills of the present invention

[0035] 1) Preparation of the test product solution in the fat-soluble part: take Xiaojin pills and crush them into fine powder, weigh 0.6g precisely, add 5mL ether, ultrasonicate for 30min, filter, add 3mL ether to the filter residue, ultrasonically 15min, filter, wash the filter residue with 2mL ether, and combine the filtrates , evaporate the solvent at 40°C, add methanol to dissolve the residue, dilute the methanol to 5mL, pass through a 0.22μm filter membrane, and obtain the product;

[0036] 2) draw need testing solution and inject high-performance liquid chromatograph, and chromatographic condition is as follows:

[0037] Chromatographic column: Welch UltiMate AQ-C18 (4.6×250mm); detection wavelength: 202nm; injection volume is 15ul, flow rate is 1ml / min, column temperature is 30°C; mobile phase: acetonitrile as mobile phase A, 0.1% Phosphoric acid solution is mobi...

Embodiment 2

[0041] Embodiment 2 Fingerprint detection of water-soluble parts of Xiaojin pills of the present invention

[0042] 1) Preparation of the water-soluble part of the test solution: take the filter residue of step 2) of Example 1, evaporate the residual ether, add 5 times the amount (v / w; mL / g) of 70% ethanol, ultrasonic 30min, centrifuge, take the The clear liquid was passed through a 0.22 μm filter membrane;

[0043] 2) Draw the water-soluble part for the test product solution and inject it into the high-performance liquid chromatograph, and the chromatographic conditions are as follows:

[0044] Chromatographic column: chromatographic column is Welch UltiMate AQ-C18 (4.6×250mm); detection wavelength: 250nm; injection volume is 15ul, flow rate is 1ml / min, column temperature is 30°C; mobile phase: acetonitrile as mobile phase A, Use 0.1% phosphoric acid solution as mobile phase B; the gradient elution procedure is as follows:

[0045]

[0046]

[0047] 3) The fingerprints ...

experiment example 1

[0050] 1. Instrument

[0051] Thermo Scientific UltiMate 3000 high-performance liquid chromatography, Welch UltiMate AQ-C18 chromatographic column (4.6 × 250mm).

[0052] 2. Reagents

[0053] Chromatographic acetonitrile, UP ultrapure water, phosphoric acid, ether, chromatographic grade methanol, pure ethanol.

[0054] 3. Liquid chromatography system conditions

[0055] Gradient elution is adopted, the mobile phase A is 0.1% phosphoric acid aqueous solution, the mobile phase B is acetonitrile, the elution time of the fat-soluble part is 80 minutes, the elution time of the water-soluble part is 58 minutes, and the flow rate is 1.0ml / min; the column temperature is 30 °C; The ultraviolet detection wavelength of the soluble part is 202nm, and the ultraviolet detection wavelength of the water-soluble part is 250nm;

[0056] Gradient elution program for fat-soluble parts: 0-5min, 40% acetonitrile; 5-10min, 40%-50% acetonitrile; 10-20min, 50%-60% acetonitrile; 20-30min, 60%-65% ac...

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Abstract

The invention discloses a Xiaojin pill fingerprint detection method. According to the method, fat-soluble components are separated from water-soluble components of Xiaojin pills, two fingerprints areestablished for the two parts respectively, a double-part double-wavelength quality control idea is used to control the overall quality of the Xiaojin pills, and thus, the quality standard system of the Xiaojin pills is improved and the clinical curative effect is guaranteed.

Description

technical field [0001] The invention relates to the technical field of traditional Chinese medicine fingerprints, in particular to a method for detecting the fingerprints of Xiaojin Pills. Background technique [0002] Xiaojin Wan has the effects of dispelling stagnation, reducing swelling, removing blood stasis and relieving pain. It is mainly used clinically to treat scrofula, goiter, breast rock, breast addiction and other syndromes caused by stagnation of phlegm and qi. It is the preferred Chinese patent medicine for the clinical treatment of mammary gland hyperplasia in contemporary Chinese medicine. In recent years, with the deepening of pharmacological research, the scope of applicable diseases of Xiaojin Pills has expanded. Hepatitis fibrosis has a good therapeutic effect. [0003] The prescription of Xiaojinwan is complicated, and the whole prescription is composed of 10 medicinal materials, including musk, wood turtle, aconitum, maple balm, vinegar frankincense, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/86
CPCG01N30/02G01N30/8686
Inventor 韩丽冯碧张定堃宋娇
Owner CHENGDU UNIV OF TRADITIONAL CHINESE MEDICINE
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