高效液相色谱-质谱法测定牛奶中6 种氨基甲酸酯农药残留[J].pdf

※分析检测 食品科学 2011, Vol. 32, No. 02 18 7 高效液相色谱- 质谱法测定牛奶中 6 种氨基甲酸酯农药残留 田宏哲，赵瑛博，周艳明 (沈阳农业大学分析测试中心，辽宁沈阳 110866) 摘 要：为建立同时测定牛奶中6 种氨基甲酸酯类农药残留量的方法，样品经乙腈提取，Oasis HLB 固相萃取柱净 化后，采用高效液相色谱- 离子阱质谱(HPLC-ESI-MS/MS)进行测定，测定条件为：C18 色谱柱分离，甲醇-0.02mol/L 醋酸铵溶液梯度洗脱，多反应监测模式检测。结果表明，6 种杀虫剂的定量限为1.0～10 .0 μg/k g ，平均添加回收 率为79.2 1%～9 1.38% ，相对标准偏差为3.44%～5.7 1% 。本实验所建立的6 种杀虫剂的测定方法完全可以满足当前 农药残留分析的要求。 关键词：高效液相色谱- 电喷雾电离质谱；杀虫剂；氨基甲酸酯农药；牛奶 Simultaneous Determination of Six Carbamate Pesticide Residues in Milk by HPLC-ESI-MS/MS TIAN Hong-zhe ，ZHAO Ying-bo ，ZHOU Yan-ming (Analysis and Testing Center, Shenyang Agricultrual University, Shenyang 110866, China) Abstract ：A high performance liquid chromatography-ion trap mass spectrometric (HPLC-ESI-MS/MS) method was developed to determine six carbamate pesticide residues in milk samples simultaneously. Samples were extracted with acetonitrile, cleaned up on an Oasis HLB-SPE column, separated on a C18 column using mixed methanol and 0.02 mol/L ammonium acetate as a mobile phase (60:40, V/ V) by gradient elution, followed by multiple reaction monitoring (MRM) mode detection. The limits of quantification ranged from 1.0 to 10.0 μg/kg. The average recoveries in spiked samples were between 79.2 1% and 9 1.38% with relative standard deviation s from 3.44% to 5.7 1%. The proposed method can meet the current requirements for the analysis residual pesticides. Key words：high performance liquid chromatography-electrospray ionization mass spectrometry ；in sectcide；carbamate pesticide residue；milk 中图分类号：O654.7 文献标识码：A 文章编号：1002-6630(20 11)02-0 187-04 由于氨基甲酸酯类农药是一类高效、低毒的广谱杀 复杂；化学发光法和液相色谱- 紫外法检测灵敏度较