Determination method for arsanilic acid, nitarsone and roxarsone in animal foodstuff

Abstract

The invention provides a determination method for arsanilic acid, nitarsone and roxarsone in an animal foodstuff. The invention is characterized in that the determination method comprises the following steps: weighing A g of a to-be-determined sample, placing the sample in a mortar, adding 3A g of Florisil, carrying out full mixing with stirring, using an accelerated solvent extraction instrument for extraction, wherein an aqueous methanol solution with a volume ratio of methanol to water of 3: 7 is used as an extraction solvent, and allowing a constant volume of 5A ml to be obtained through addition of water after completion of extraction; and carrying out filtering with a filter membrane and carrying out determination by using liquid chromatography-atomic fluorescence spectroscopy; wherein A is an integer not equal to zero. Compared with the prior art, the invention has the following advantages: the method for simultaneous determination of residual quantities of arsanilic acid, nitarsone and roxarsone in animal derived food by using accelerated solvent extraction-liquid chromatography-atomic fluorescence spectroscopy is researched and established in embodiments in the invention; the proportion of the extraction solvent, extraction temperature, extraction time and extraction frequency of accelerated solvent extraction technology are optimized, and the advantages of a small usage amount of the extraction solvent, rapidness, small influence on a matrix, high extraction efficiency and good selectivity are obtained.

Description

technical field [0001] The invention relates to a method for determining the residues of arsanic acid, nitrophenyl arsenic acid and roxarsine in animal-derived food. Background technique [0002] In recent years, organic arsenic preparations have been widely used in the world as feed additives for anti-pathogenic microorganisms and growth-promoting animals. The main types are arsanic acid (ASA), roxarsarsenic acid (ROX), and nityl arsenic acid (NIT). [0003] In the prior art, the detection methods about them are mainly chromatographic and detector combined technology: such as adopting high-performance liquid chromatography-ultraviolet detector to measure arsanic acid, nitrophenyl arsenic acid and roxarsarsenic in the feed, but this The method is only applicable to the detection of feed samples; [0004] Another example is the liquid chromatography-mass spectrometry method for the determination of organic arsenic veterinary drugs with low detection limit, low solvent consu...

AI Technical Summary

Problems solved by technology

However, due to its high price and high operating cost, it is difficult to popularize at present, and the salt content in the sample has great interference on the determination of arsenic by ICP-MS

In addition, the mobile phase of HPLC usually contains a certain proportion of organic solvents. The carbon generated by organic solvents in ICP can cause the ICP-MS injection tube to be blocked and the holes of the sampling cone and skimmer cone to become smaller and smaller. Even blocked, resulting in unstable ICP-MS signal;

[0005] Another example is the existing improved scheme, which uses liquid chromatography-hydride generation-atomic fluorescence to detect simultaneously. The arsenic compound has a good linear relationship with the fluorescence peak area within a certain concentration range, but this type of scheme is not suitable for complex matrices. The solvent extraction and extraction efficiency of the sample are low, therefore, it is necessary to further improve the determination method of arsanic acid, nitrophenyl arsenic acid and roxarsine residues in food of animal origin

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