高效液相色谱-串联质谱法检测橘子中10种氨基甲酸酯类农药残留  

Determination of Multi-residues for 10 Carbamate Pesticides by HPLC Coupled with Mass Spectrometry

作　　者：刘旭凌[1] 李壹[2] 熊晓辉[2] 

机构地区：[1]南京工业大学生物与制药工程学院,南京211816 [2]南京工业大学食品与轻工学院,南京211816

出　　处：《科学技术与工程》2015年第9期10-14,38,共6页Science Technology and Engineering

基　　金："十二五"国家科技计划项目(2012BAK17B09);江苏省科技基础设施建设计划(BM2012026)资助

摘　　要：为建立高效液相色谱-串联质谱（LC-MS/MS）同时测定橘子中10种氨基甲酸酯类农药残留量的方法,以橘子样品经简单前处理后,以乙腈-0.05%甲酸水为流动相,经赛默飞C18色谱柱（3.0×100 mm,2.2μm）梯度洗脱,柱温35℃,进样量为10μL,采用串联三重四级杆质谱多反应监测（MRM）正离子模式进行检测。对整个测量过程的不确定度来源进行了分析,并对不确定度各个分量进行了评定和合成。结果 10种氨基甲酸酯类农药残留在0-100μg/kg范围内线性良好,相关系数均大于0.992,在10、50、100μg/kg 3个加标水平下加标回收率分别是：61.08%-93.88%;79.22%-114.82%;82.82%-124.67%;10μg/kg加入量的变异系数（CV）为1.21%-15.03%,重复性测量不确定度显示准确性较高,达国家相关标准规定。该方法简便、快速、灵敏,适用于橘子中氨基甲酸酯类农药残留的分析检测。To establish a method for the determination of 10 Carbamate Pesticides in orange by LC-MS /MS,the samples were separated by using a linear solvent acetonitrile-water（ containing 0.05% formic acid） gradient after simple pretreated.The column was Thermo C18（ 3.0 × 100 mm,2.2 μm）,the temperature was 35 ℃ and the injection volume was 10 μL.The samples were detected by triple quadrupole with multiple reaction monitoring（ MRM） in positive mode.The sources of uncertainty of the measurement progress were analyzed,and the uncertainty of each component was evaluated and calculated.Results 10 carbamate pesticide residues showed good linear relationship in 0 ~ 100 μg / kg,with the correlation coefficients of greater than 0.992.The recoveries for all 10 analytes in 3 different degrees： 10 μg / kg ranged from 61.08% ~ 93.88%; 50 μg / kg： 79.22% ~ 114.82%; 100μg /kg： 82.82% ~ 124.67%.The CV（ coefficient of variation） of 10 μg /kg ranged from 1.21% ~ 15.03%.Repeatability measurement uncertainty shows high accuracy that reaches relevant national standards.The method is simple,rapid,accurate and suitable for simultaneous determination of these pesticides in orange.

关 键 词：高效液相色谱-串联质谱(LC-MS/MS) 农药残留 氨基甲酸酯类 

分 类 号：O657.63[理学—分析化学]