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Determination method of benzimidazoles drug residues in chicken tissues

The technology of a benzimidazole and a determination method is applied in the field of determination of the residual amount of benzimidazoles in chicken tissue, and can solve problems such as technical difficulties and the like

Active Publication Date: 2018-12-14
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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  • Determination method of benzimidazoles drug residues in chicken tissues
  • Determination method of benzimidazoles drug residues in chicken tissues
  • Determination method of benzimidazoles drug residues in chicken tissues

Examples

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 a determination method of benzimidazoles drug residue in chicken, chicken liver and chicken kidney. The determination method comprises the step of simultaneously determining residues ofnine benzimidazoles drug residual markers in the chicken, chicken liver and chicken kidney by adopting high-performance liquid chromatography, and the technical blank at this field is filled. A regression equation related coefficient of the method reaches 0.999 and more, the lower determination limit is 50 micrograms / kg, the recovery rates on different adding concentration levels are 75%-110%, andthe relative standard deviation in the experiment is not more than 15%. The technical problem of simultaneously determining nine benzimidazoles drugs is solved, the determination has the originalityon the pre-treatment technology of the sample, especially on the purification technology. The method is scientific and accurate in quantification, strong in interference resistance, wide in matrix adaption range, and capable of satisfying the latest technical requirement of the related supervision department of our 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 Applications(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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