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Simultaneously Quantification of Ethanamizuril Marker Residue in Edible Tissues of Chicken by Ultra-high Performance Liquid Chromatography–Mass Spectrometry
Food Analytical Methods ( IF 2.6 ) Pub Date : 2019-11-16 , DOI: 10.1007/s12161-019-01669-3
Yingchun Liu , Xiao Zhao , Chunmei Wang , Keyu Zhang , Lifang Zhang , Mi Wang , Chenzhong Fei , Xiaoyang Wang , Feiqun Xue

Abstract

Ethanamizuril (EZL) is a novel anti-coccidiosis triazine compound synthesized in our laboratory. The marker residue of EZL in chicken tissues was EZL and its metabolite deacetylethanamizuril (deacetylEZL). In order to quantitatively analyze the EZL and deacetylEZL in chicken tissues, a rapid, simple, and specific ultra-high-performance liquid chromatography–mass spectrometry (UPLC-MS/MS) method was developed. Validation was performed according to the European Commission Decision 2002/657/EC guidelines. The detection limit was 5 μg kg−1, 10 μg kg−1, and 5 μg kg−1 in muscle, liver, and skin+fat for EZL. And the detection limit of deacetylEZL was 2 μg kg−1, 10 μg kg−1, 2 μg kg−1, and 10 μg kg−1 in muscle, liver, skin+fat, and kidney, respectively. The mean recoveries from fortified samples ranged from 80.15 to 99.50%, with inter assay coefficients of variation ranging between 5.03 and 15.84%. Based on this method, the depletion profile of EZL was studied in 60 healthy chickens after administration of 10 mg L−1 via drinking water for 3 days. Six medicated and one control chicken were sacrificed at 4, 8, 12, 24, 48, 60, 72, 96, and 120 h after the cessation of treatment. The highest residue concentrations of marker residue were attained at the first day, and those of all samples were below the MRL at 68.74 h post-treatment. The concentration of marker residue in kidney tissue was significantly higher than those in liver, skin+fat, and muscle tissues. The statistically estimated withdrawal period of EZL with oral administration was 4 days.



中文翻译:

高效液相色谱-质谱法同时定量分析鸡肉中可食性乙胺嘧啶标记残留

摘要

乙胺嘧啶(EZL)是在我们的实验室中合成的新型抗球虫三嗪化合物。鸡组织中EZL的标志残基是EZL及其代谢物脱乙酰乙胺嘧啶(deacetylEZL)。为了定量分析鸡肉组织中的EZL和脱乙酰基EZL,开发了一种快速,简单且特异的超高效液相色谱-质谱(UPLC-MS / MS)方法。验证根据欧盟委员会的决定进行2002年/ 657 / EC准则。检测极限为5μg千克-1,10微克千克-1,和5μg千克-1在肌肉,肝脏和皮肤+脂肪EZL。和deacetylEZL的检出限为2微克千克-1,10微克千克-1,2微克公斤-1和10μgkg -1分别在肌肉,肝脏,皮肤+脂肪和肾脏中。强化样品的平均回收率在80.15%至99.50%之间,测定间变异系数在5.03%至15.84%之间。基于此方法,研究了60 mg健康鸡在服用10 mg L -1后的EZL消耗情况通过饮用水3天。在停止治疗后第4、8、12、24、48、60、72、96和120小时处死6只药鸡和1只对照鸡。在第一天就达到了标记残留的最高残留浓度,并且所有样品的残留浓度在处理后68.74 h均低于MRL。肾脏组织中标志物残留的浓度显着高于肝脏,皮肤+脂肪和肌肉组织中的残留。经统计学估计,口服EZL的停药期为4天。

更新日期:2020-01-23
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