高效液相色谱-电感耦合等离子体质谱同时分析鸡肉中洛克沙生、阿散酸和硝苯胂酸

摘要

An analytical method was developed to simultaneously determine roxarsone,arsanilic and nitarsone in chicken by high performance liquid chromatography/inductively coupled plasma mass spectrometry（HPLC-ICP-MS）.Samples were extracted with methanol/water solution.The chromatographic separation was performed on a Phenomenex Luna C18 using methanol and water（containing 0.05% trifluoroacetic acid） as the mobile phase.Identification and quantification were achieved by using ICP-MS.Good linearity was observed in the range of 1 to 50 μg/kg with correlation coefficients above 0.99.The method was validated at the spike levels of 1,2,10 μg/kg.The validation results indicated that the average recoveries of arsenicum praeparatum ranged from 85.4% to 103.1% with a relative standard deviation of 3.3%-7.2%.The quantification limits of 3 arsenicum praeparatum were 1μg/kg.The method had good reproducibility,high sensitivity and simple pre-treatment.Its performance could meet both domestic and international legislation requirements.This method is applicable for simultaneous determination of arsenicum praeparatum in chicken.%建立一种同时测定鸡肉中洛克沙生、阿散酸和硝苯胂酸等3种有机砷类制剂的高效液相色谱-电感耦合等离子体质谱（high performance liquid chromatography tandem inductively coupled plasma mass spectrometry,HPLC-ICP-MS）分析方法。样品经甲醇溶液提取,采用Phenomenex Luna C18色谱柱,体积分数0.05%的三氟乙酸溶液-甲醇作为流动相进行洗脱,经高效液相色谱分离,电感耦合等离子体质谱进行定性和定量分析。结果表明：1～50μg/kg范围内各砷制剂线性良好,相关系数r2均在0.99以上;在1、2、10μg/kg三个加标水平下进行方法验证,平均回收率为85.4%～103.1%,相对标准偏差为3.3%～7.2%;3种有机砷类制剂的定量限均为1μg/kg。方法重现性好、灵敏度高、前处理简单,各项指标均满足国内外法规要求,适用于鸡肉中有机砷类制剂残留的分析检测。