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Method for analyzing amitraz residual marker

A marker and formamidine technology, which is applied in the field of detection of formamidine residue markers and achieves the effect of high detection sensitivity

Inactive Publication Date: 2013-12-04
HUAZHONG AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At home and abroad, most studies are on the detection method of amitraz residues in bee products, and the research on residue detection methods in animal edible tissues is basically blank.

Method used

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  • Method for analyzing amitraz residual marker
  • Method for analyzing amitraz residual marker
  • Method for analyzing amitraz residual marker

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: Derivatization reaction of formamidine residue markers with heptafluorobutyric anhydride

[0035] (1) Amitraz and 2,4-dimethylaniline react with heptafluorobutyric anhydride

[0036] Accurately weigh an appropriate amount of amitraz and 2,4-dimethylaniline standard substances, dilute them with n-hexane, and prepare the concentrations of 10 μg / L, 20 μg / L, 50 μg / L, 100 μg / L, 200 μg / L, 400μg / L, 800μg / L mixed standard solution. Measure the mixed standard solution into a polypropylene centrifuge tube, add 10 mL of alkaline aqueous solution (take 1000 mL of distilled water, adjust the pH value to 9.0 with 1 mol / L sodium hydroxide solution), vortex to mix, and centrifuge at 4200 r / min for 10 min. Transfer the supernatant to a polypropylene centrifuge tube, repeat the extraction once, and combine the two extracts. Stand for hydrolysis in a constant temperature drying oven at 70°C for 50 minutes. After cooling, add 5.0 mL of n-hexane to the extract, vortex to mix, ...

Embodiment 2

[0053] Embodiment 2: the mensuration of sample

[0054] (1) Extraction of samples

[0055] The fat, liver, and kidney tissues of pigs, cattle, and sheep were selected as experimental samples, and the residues of amitraz and its metabolite 2,4-dimethylaniline were detected. There are 3 additive concentrations: 20μg / L, 200μg / L, and 400μg / L for fat, liver, and kidney tissues of cattle; 20μg / L, 400μg for fat, liver, and kidney tissues of pigs, cattle, and sheep, respectively. / L and 800μg / L, and set a blank sample respectively. Including three concentrations of limit of quantitation and Chinese meaning (MRL) and 2MRL, each concentration has 5 repeated samples, measured 3 times at different times, and the recovery rate is calculated by the external standard method (reference).

[0056] Weigh (5±0.05) g of the above-listed test materials into a polypropylene centrifuge tube, add 10 mL of alkaline distilled water, vortex and mix, centrifuge at 4200 r / min for 10 min, transfer the su...

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Abstract

The invention belongs to a method for analyzing an amitraz residual marker, and particularly relates to an analytic method for derivatization reaction of an amitraz residual marker (heptafluorobutyric anhydride) and gas chromatography detection and simultaneous detection. The amitraz residual marker and heptafluorobutyric anhydride can react to obtain a fluorine-containing product which is easier to gasify and has a stronger detection signal. The reaction conditions are optimized, under the alkaline condition, in a thermostatic drying cabinet at the temperature of 65-75 DEG C, an amitraz compound is hydrolyzed for 40-60 min; in a thermostatic drying cabinet at the temperature of 55-75 DEG C, the amitraz hydrolysis product and heptafluorobutyric anhydride react for 80-100 min, after the cooling to the room temperature, saturated NaHCO3 is added for neutralization, and the gas chromatography analysis is directly carried out after the drying. The minimum detectable amount is 5 [mu]g / L, the reproducibility of results is good, three concentrations are obtained, the 5-time independently repeated coefficients of variation are less than 15%, and all indexes can meet the analysis requirement for drug residual quantity.

Description

technical field [0001] The invention belongs to the technical field of veterinary drug residue analysis, and in particular relates to a detection method for formamidine residue markers. The invention can be used to detect the residues of dipinamidine and its residue markers in animal foods. Background technique [0002] Amitraz belongs to the formamidine class of insecticides. It is a new type of moderately toxic acaricide, which is effective in preventing and controlling lice mites in pigs, cattle and sheep. EU 2377 / 90EEC stipulates that veterinary drug residues in animal foods include drug prototypes and various active ingredients, metabolites, and degradation products. Amitraz is easily degraded into the intermediate product monoformamidine in the environment and living animals (FAO / WHO1985; Knowles and Hamed, 1989; Pass and Mogg, 1991; Konopka1994; Pass and Mogg1995; Corta et al.1999). Amitraz mainly stimulates adrenergic receptors, causing impairment of consciousness,...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 袁宗辉陶燕飞陈冬梅潘源虎黄玲利王玉莲王旭刘振利谢叔宇彭大鹏戴梦红郝海红程古月
Owner HUAZHONG AGRI UNIV
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