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Method for Enrichment and Detection of Trace Aristolochic Acid A from Longdan Xiegan Pills

A technology for gentian xiegan pills and aristolochic acid, which is applied to measurement devices, instruments, analytical materials, etc., can solve the problems of difficult elution, large loss of imprinted polymers, limited binding capacity, etc., and achieves a safe enrichment process. , The operation process is simple, and the effect of reducing toxic damage

Active Publication Date: 2019-06-28
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The bulk imprinted polymer obtained by bulk polymerization often needs to be crushed, ground, and sieved before it can be used. The processing process is complex and time-consuming, and the imprinted polymer is lost during the sieving process. The shape of the product is irregular and the dispersion is poor.
The in-situ polymerization method is to directly synthesize a continuous porous imprinted polymer in the column tube, but the column efficiency is still not high, and there is a problem of high column pressure
In addition, the synthesized imprinted polymer embeds template molecules too deeply and tightly, resulting in difficulty in elution, limited binding capacity, high diffusion resistance of template molecules, slow mass transfer rate, and difficulty in identifying sites for binding, which leads to the difficulty in practical applications. Low enrichment efficiency of template molecules

Method used

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  • Method for Enrichment and Detection of Trace Aristolochic Acid A from Longdan Xiegan Pills
  • Method for Enrichment and Detection of Trace Aristolochic Acid A from Longdan Xiegan Pills
  • Method for Enrichment and Detection of Trace Aristolochic Acid A from Longdan Xiegan Pills

Examples

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Embodiment 1

[0028] Embodiment 1, with reference to figure 1 A method for enriching and detecting trace amounts of aristolochic acid A from the Chinese patent medicine Longdan Xiegan Pills, comprising the following steps:

[0029] 1) Preparation of molecularly imprinted polymers:

[0030] 1.1) Activation of silica gel:

[0031] Weigh 30g of silica gel, add it to 250mL of dilute hydrochloric acid with a mass concentration of 10%, heat and reflux at 110°C for 24h; filter and wash with ultrapure water until neutral, then dry at 55°C for 24h to obtain activated silica gel for use;

[0032] 1.2) Surface modification of silica gel:

[0033] Weigh 30g of activated silica gel, add the first mixed solution consisting of 50mL toluene, 2mL APTES and 1mL triethylamine to form a mixed system, heat the mixed system at 110°C for 24h, wash with methanol suction filtration until neutral, and dry at 55°C for 24h , to obtain modified silica gel for subsequent use;

[0034] 1.3) Synthesis of molecularly i...

Embodiment 2

[0041] Example 2, a method for enriching and detecting trace amounts of aristolochic acid A from the Chinese patent medicine Longdan Xiegan Pills, comprising the following steps:

[0042] 1) Preparation of molecularly imprinted polymers:

[0043] 1.1) Activation of silica gel:

[0044]Weigh 25g of silica gel, add it to 250mL of dilute hydrochloric acid with a mass concentration of 10%, heat and reflux at 110°C for 24h; filter and wash with ultrapure water until neutral, then dry at 55°C for 24h to obtain activated silica gel for use;

[0045] 1.2) Surface modification of silica gel:

[0046] Weigh 30g of activated silica gel, add the first mixed solution consisting of 100mL toluene, 4mL APTES and 1mL triethylamine to form a mixed system, heat the mixed system at 110°C for 24h, filter and wash with methanol until neutral, and dry at 55°C for 24h , to obtain modified silica gel for subsequent use;

[0047] 1.3) Synthesis of molecularly imprinted polymers on the surface of sil...

Embodiment 3

[0054] Example 3, a method for enriching and detecting trace amounts of aristolochic acid A from the Chinese patent medicine Longdan Xiegan Pills, comprising the following steps:

[0055] 1) Preparation of molecularly imprinted polymers:

[0056] 1.1) Activation of silica gel:

[0057] Weigh 40g of silica gel, add it to 250mL of dilute hydrochloric acid with a mass concentration of 10%, heat and reflux at 110°C for 24h; filter and wash with ultrapure water until neutral, then dry at 55°C for 24h to obtain activated silica gel for use;

[0058] 1.2) Surface modification of silica gel:

[0059] Weigh 30g of activated silica gel, add the first mixed solution consisting of 50mL toluene, 3mL APTES and 1mL triethylamine to form a mixed system, heat the mixed system at 110°C for 24h, filter and wash with methanol until neutral, and dry at 55°C for 24h , to obtain modified silica gel for subsequent use;

[0060] 1.3) Synthesis of molecularly imprinted polymers on the surface of sil...

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Abstract

The invention discloses a method for enriching and detecting trace aristolochic acid A in a traditional Chinese medicine bolus of gentian for purging liver-fire. The method comprises the following steps: firstly, activating silica gel; then modifying a surface of the silica gel; synthesizing a molecularly imprinted polymer on the surface of the silica gel; filling a column with the molecularly imprinted polymer; activating with methanol to obtain a molecularly imprinted solid phase extraction column; using the molecularly imprinted solid phase extraction column for detecting and enriching aristolochic acid A in the traditional Chinese medicine bolus of gentian for purging liver-fire. The method provided by the invention has advantages of simple operation, high binding capacity, high mass transfer rate and high enrichment efficiency.

Description

technical field [0001] The invention relates to the technical field of molecular imprinting, in particular to a method for enriching and detecting trace amounts of aristolochic acid A from Longdan Xiegan Pills, a Chinese patent medicine. Background technique [0002] Aristolochic acid A is a class of nitrophenanthrene compounds, mainly found in plants of the genus Aristolochia and Asarum, which can cause severe nephrotoxicity. Medicinal plants and preparations containing aristolochic acids have been successively Banned in many countries. At present, some traditional Chinese medicines and related Chinese patent medicines are still in use, and the removal of aristolochic acid in Chinese medicines is beneficial to reduce the toxicity of Chinese medicines. [0003] At present, there are two commonly used enrichment methods for aristolochic acid A: solvent method column separation method; solid phase extraction method, among the above enrichment methods for aristolochic acid A: ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/08C08F292/00C08F220/06C08F222/14C08J9/26
CPCC08F292/00C08J9/26C08J2201/0424C08J2351/10G01N30/02G01N30/08C08F220/06
Inventor 傅强葛燕辉余佩舒花常春曾爱国
Owner XI AN JIAOTONG UNIV
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