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A kind of assay method of benzimidazole drug residue in chicken tissue

A technology of benzimidazole and determination method, which is applied in the field of determination of benzimidazole drug residues in chicken tissue, and can solve technical difficulties and other problems

Active Publication Date: 2021-04-27
INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Benzimidazoles are generally weakly alkaline due to their chemical structure, but the residual marker triclabendazole, triclabendazole, is a neutral compound. I want to detect these nine benzimidazoles at the same time There are many technical difficulties in the residue markers of drugs, especially the use of high performance liquid chromatography, which has higher requirements for sample purification

Method used

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  • A kind of assay method of benzimidazole drug residue in chicken tissue
  • A kind of assay method of benzimidazole drug residue in chicken tissue
  • A kind of assay method of benzimidazole drug residue in chicken tissue

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1: Establishment method

[0037] 1. Reagents and Materials

[0038] The reagents used below are all analytical reagents unless otherwise specified; the water is first-class water in accordance with GB / T 6682.

[0039] Standard: Oxfendazole (CAS No.: 53716-50-0), Fenbendazole (CAS No.: 43210-67-9), Oxfendazole-2-aminosulfone (Oxfendazole sulphone, CAS No.: 54029-20-8), Albendazole-2-aminosulfone (Albendazole-2-aminosulfone, CAS No.: 80983-34-2), Thiabendazole (CAS No.: 148-79- 8), 5-hydroxythiabendazole (5-hydroxythiabendazole, CAS number: 948-71-0), 2-amino-5-benzoylbenzimidazole (Mebendazole-amine, CAS number: 52329-60-9 ), 5-Hydroxymebendazole (5-Hydroxymebendazole, CAS No.: 60254-95-7), Flubendazole (Flubendazole, CAS No. 31430-15-6), Oxibendazole (Oxibendazole, CAS No.: 20559 -55-1) and triclabendazole (Ketotriclabendazole, CAS No.: 1201920-88-8), the content of which is above 97%.

[0040] Acetonitrile: chromatographically pure; methanol: chromatographi...

Embodiment 2

[0111] Embodiment 2: the selection of extraction solvent

[0112] The present invention compares acetonitrile and the basic ethyl acetate used in GB / T 21324-2007 "Methods for the Detection of Benzimidazole Drug Residues in Edible Animal Muscle and Liver". Under the chromatographic system conditions of the method, acetonitrile extracts The interference peaks of the liquid are far less than that of basic ethyl acetate. In addition, the basic ethyl acetate extract must be converted to solvent before being purified and put on the column in the next step. 0.1mol / L hydrochloric acid solution is dissolved, and the concentration process will cause the degradation of triclabendazolone, while the acetonitrile extract does not need to be concentrated, and can be loaded on the column after adding 0.1mol / L hydrochloric acid solution. The extraction efficiency of all the compounds in the acetonitrile extraction liquid reaches more than 95%, so the present invention selects acetonitrile as t...

Embodiment 3

[0113] Embodiment 3: the selection of purification conditions

[0114] At first, the present invention tries to adopt reverse-phase adsorbent HLB solid-phase extraction small column, when the acetonitrile ratio in the upper column solution is 10%, oxfendazole-2-aminosulfone and 5-hydroxythiabendazole will be lost to some extent, Therefore, the acetonitrile extract must be concentrated, which will not only cause the degradation of the compound to be tested, but also cause the proportion of organic solvent to be too low during re-dissolution, resulting in poor dissolution effect and lower recovery rate.

[0115] After comparison, this method adopts MCX solid-phase extraction small column, for triclabendazolone, the N-vinylpyrrolidone-divinylbenzene copolymer in the filler has played the effect of reverse phase adsorbent; As far as the compound is concerned, the N-vinylpyrrolidone-divinylbenzene copolymer matrix-SO3H in the filler mainly plays the role of ion exchange. Combining...

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Abstract

The invention discloses a method for determining the residual amount of benzimidazoles in chicken, chicken liver and chicken kidney. The present invention provides for the first time the simultaneous determination of the residues of nine benzimidazole drug residue markers in chicken, chicken liver and chicken kidney by using high performance liquid chromatography, which fills the technical gap in the art. The correlation coefficient of the regression equation of the present invention reaches more than 0.999, the lower limit of determination is 50 μg / kg, the recovery rate at different concentration levels is 75% to 110%, and the relative standard deviation in the laboratory is ≤15%. The present invention solves the technical problem of simultaneous determination of nine kinds of benzimidazole drugs, and has originality in the sample pretreatment technology, especially in the purification technology. Meet the latest technical requirements of relevant regulatory authorities in my country.

Description

technical field [0001] The invention belongs to the technical field of detection of veterinary drug residues in food, and in particular relates to a method for measuring the residues of benzimidazoles in chicken tissues. Background technique [0002] my country's latest "National Food Safety Standard Maximum Residue Limits of Veterinary Drugs in Animal Foods" (Draft for Comment) stipulates benzimidazole drugs, including febantyr, fenbendazole, oxfendazole, and oxybenzone Residue markers of thiabendazole, thiabendazole, triclabendazole, albendazole, flubendazole and mebendazole. There are many differences from the previous Ministry of Agriculture Announcement No. 235. First, the types of drugs have been increased and the names have been standardized. Secondly, the residue markers have also been greatly revised. The residue marker of febantyr / fenbendazole / oxfendazole is the sum of fenbendazole, oxfendazole and oxfendazole 2-aminosulfone; Bendazole; the residue markers of thia...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 邵琳智吴映璇林峰欧阳少伦蓝草陈思敏
Owner INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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