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Method for discriminating donkey-hide gelatin utilizing liquid-liquid-liquid three phase static extracting efficient liquid-phase chromatograph

A technology of high performance liquid chromatography and static extraction, which is applied in the field of liquid-liquid-liquid three-phase static extraction high performance liquid chromatography to identify donkey-hide gelatin, which can solve the problem that the authenticity of donkey-hide gelatin is difficult to judge, the separation effect cannot be achieved, and the separation effect is not good. And other issues

Inactive Publication Date: 2007-12-05
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the spectroscopic method does not have the separation function, the measured spectrum of the mixture is a superimposed spectrum. The more components and the more complex, the simpler the spectral information obtained. It is used for the identification of donkey-hide gelatin and other glues, and the identification features are not obvious.
Although chromatography has the function of separation, for the complex composition system of donkey-hide gelatin, the existing sample pretreatment method and chromatographic conditions cannot achieve the ideal separation effect
If the separation effect is not good, a small number of characteristic components will be covered by many non-characteristic components, and the chromatograms of the tested gelatin will be very similar, and it will be difficult to judge the authenticity of donkey-hide gelatin.

Method used

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  • Method for discriminating donkey-hide gelatin utilizing liquid-liquid-liquid three phase static extracting efficient liquid-phase chromatograph
  • Method for discriminating donkey-hide gelatin utilizing liquid-liquid-liquid three phase static extracting efficient liquid-phase chromatograph
  • Method for discriminating donkey-hide gelatin utilizing liquid-liquid-liquid three phase static extracting efficient liquid-phase chromatograph

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Experimental program
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Effect test

Embodiment 1

[0053] The mensuration of the donkey-hide gelatin HPLC collection of illustrative plates of embodiment 1

[0054] 1 Instruments and reagents

[0055] 1.1 Instrument

[0056] Agilent 1100 high performance liquid chromatography; Agilent DAD diode array ultraviolet detector; Agilent ChemStation.

[0057] 1.2 Reagent

[0058] DL-β-phenylalanine, DL-tyrosine, and bilirubin reference substance, chromatographically pure, were purchased from Shandong Pharmaceutical Company; quercetin standard substance was purchased from China Institute for the Control of Pharmaceutical and Biological Products; acetonitrile (imported ), chromatographically pure; high-purity water; chloroform, n-hexane, and absolute ethanol are all analytically pure; donkey-hide gelatin, yellow gelatin, and miscellaneous hide glue are provided by Liaocheng Drug Control Institute of Shandong Province.

[0059] 2 Chromatographic conditions

[0060] The chromatographic column packing is octadecylsilane bonded silica gel...

Embodiment 2

[0104] The determination of embodiment 2 donkey-hide gelatin HPLC collection of illustrative plates

[0105] Except that it is different from 3.1.2 extraction in Example 1, all the others are the same.

[0106] The extraction method of Example 2 is as follows: put the dissolved mesophase solution in a 50ml conical separatory funnel, slowly add 20ml cyclohexane along the wall, seal it, and let it stand for extraction for 50 hours. After the extraction is completed, carry out phase separation, put the light phase extract on a water bath and evaporate to dryness, add absolute ethanol to dissolve the residue and set the volume to a concentration of 1g / ml, and use it as the light phase test solution of the sample; it will be extracted by the light phase solvent Slowly add the passed intermediate phase solution along the wall into another 50ml conical separatory funnel filled with 20ml of dichloromethane, seal it, and let it stand for extraction for 55 hours. After extraction, phas...

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Abstract

The present invention discloses a method adopting liquid-liquid-liquid three-phase static extraction high performance liquid chromatography to identify ass-hide glue. Said invention adopts three solvents with different polarities and different specific weights, uses non-polar solvent as light phase, the polar solvent is intermediate phase (the ass-hide glue can be previously dissolved in said phase). After the phases are separated, three polar extract test solutions are obtained, and said three test solutions are undergone the process of gradient separation by using different mobile phases, then said invention utilizes high-performance chromatography to make determination, records chromatogram and three-dimensional spectrum so as to implement identification of ass-hide glue.

Description

technical field [0001] The invention relates to the field of traditional Chinese medicine analysis. Specifically relates to a liquid-liquid-liquid three-phase static extraction method for identifying donkey-hide gelatin by high performance liquid chromatography. Background technique [0002] Donkey-hide gelatin is a well-known traditional Chinese medicine. It is a glue made from donkey skin, which is boiled and supplemented with auxiliary materials. Ejiao is mainly composed of collagen and its degradation products, such as polypeptides and various amino acids (aliphatic, basic, acidic, aromatic, heterocyclic amino acids), which have a wide range of molecular weight distribution and a large range of molecular polarity; Many other components such as sterols are difficult to carry out qualitative analysis and quality control. Mule hides, cowhide and other animal hides can also be used to make gelatin preparations. Their appearance and chemical composition are very similar to ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06B01D11/04
Inventor 程秀民
Owner SHANDONG UNIV