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Pre-column electrochemical derivatization one-time total quantity measuring method for malachite green and leucomalachite green in aquatic products

A technology of recessive malachite green and malachite green, which is applied in the direction of measuring devices, scientific instruments, instruments, etc., can solve the problem of uncontrollable amount of recessive malachite green, low accuracy of recessive malachite green, lead dioxide The problem of column unevenness and other problems can be shortened, the sample pretreatment time is shortened, the sample pretreatment is simple, and the use of reagent consumables is reduced.

Inactive Publication Date: 2016-02-03
SICHUAN ENTRY EXIT INSPECTION & QUARANTINE BUREAU INSPECTION & QUARANTINE TECHN CENT
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Problems solved by technology

However, the amount of lead dioxide is uncertain or the filled lead dioxide column is not uniform, the oxidation efficiency is uncontrollable, the amount of the recessive malachite green converted into malachite green is uncontrollable, and the detection accuracy of the recessive malachite green is not accurate. High, and weakens over time leading to poor reproducibility

Method used

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Embodiment 1

[0054] Embodiment 1, the one-time determination method of the total amount of malachite green and recessive malachite green in the aquatic products by electrochemical derivation before the column

[0055] The one-time determination method of pre-column electrochemical derivation of malachite green and recessive malachite green in aquatic products, the steps are as follows:

[0056] 1. Reagents

[0057] Standard substances: malachite green (content 98.0%); and stable malachite green (content 98.0%);

[0058] Acetonitrile (chromatographically pure, content greater than 99.9%);

[0059] Glacial acetic acid (chromatographically pure, content greater than 98%);

[0060] Anhydrous ammonium acetate (chromatographically pure, content greater than 99.9%);

[0061] Dichloromethane (chromatographically pure, content greater than 99%);

[0062] Acidic alumina solid adsorbent (particle size 50-200μm);

[0063] Sodium chloride (analytically pure, content greater than 99.8%).

[0064] ...

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Abstract

The invention provides a pre-column electrochemical derivatization one-time total quantity measuring method for malachite green and leucomalachite green in aquatic products and belongs to one-time total quantity measuring methods for converting leucomalachite green into malachite green. The key of the method is that it is found that after a leucomalachite green solution is subjected to oxidation voltage +650 mv of an electrochemical Coulomb detector (ECD), averagely 98.86% of leucomalachite green is converted into malachite green, original malachite green is unchanged, and the total concentration of leucomalachite green and malachite green can be measured through a high performance liquid chromatograph in the one-time measurement process of leucomalachite green and malachite green in a sample. Sample pre-treatment time is greatly shortened, use of reagent consumables is reduced, and electrochemical precolumn derivatization is used for replacing post-column derivatization of lead dioxide in the national standard. The method has the advantages of being simple in sample pre-treatment, good in purification effect, high in derivatization rate and high in recovery rate.

Description

technical field [0001] The invention belongs to a method for measuring malachite green and recessive malachite green, in particular to a method for one-time determination of the total amount of malachite green derivatized into malachite green before the column. Background technique [0002] Malachite Green (MalachiteGreen, MG) is a triphenylmethane chemical. It is commonly used in industry as a dye for silk, fur and paper. Since the oxidation potential of malachite green is similar to certain amino acids of pathogenic enzymes, it competes with it during cell division and hinders the formation of protein peptides, resulting in inhibition of cell division, thus playing an antibacterial and insecticidal role. Because of its obvious bactericidal effect, low price, and convenient use, it has been widely used in many countries to prevent and control saprolegniasis in aquaculture, and to kill fish ectoparasites and molds in fish eggs. The turbot food safety incident in 2006 made ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 胡江涛俞凌云吴孟茹帅培强谭志于刚张琴
Owner SICHUAN ENTRY EXIT INSPECTION & QUARANTINE BUREAU INSPECTION & QUARANTINE TECHN CENT
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