磁性多壁碳纳米管净化技术快速测定甘蓝中10种农药残留  

Simultaneous determination of ten pesticide residues in ball cabbage by ultra performance liquid chromatography-tandem mass spectrometry and magnetic multiwalled carbon nanotubes cleaning

作　　者：曹慧[1] 朱岩[2] 李祖光[3] 林静[1] 盛华栋[1] 

机构地区：[1]浙江省质量检测科学研究院浙江省食品安全重点实验室,杭州310018 [2]浙江大学化学系,杭州310028 [3]浙江工业大学化学工程与材料学院,杭州310014

出　　处：《分析试验室》2015年第12期1480-1484,共5页Chinese Journal of Analysis Laboratory

基　　金：科技部国家重大科学仪器设备开发专项(2012YQ09022903);浙江省科技厅公益性科技计划(2015C37019);浙江省质量技术监督系统科研计划(20150204)资助

摘　　要：采用磁性多壁碳纳米管-超高效液相色谱-串联质谱技术快速测定甘蓝中的10种农药残留。样品用乙腈提取，稀释后经磁性多壁碳纳米管净化，通过WatersCORTECSC18＋色谱柱分离，以甲醇和0．1％的甲酸水溶液为流动相进行梯度洗脱，采用电喷雾一正离子多反应监测模式，基质外标法定量。对磁性多壁碳纳米管的吸附时间和脱附溶剂进行考察。10种农药在相应的浓度范围内线性相关系数均大于0．99，该方法的定量限在0．3～3．0μg／kg之间。在5．0，25．0和50．0μg／kg3个浓度添加水平下，农药的回收率为80．1％～102．3％，相对标准偏差在1．9％-9．4％之间。磁性多壁碳纳米管具有较好的净化效果，适用于蔬菜中农药多残留的快速检测。A method was established for determining ten pesticide residues in ball cabbage by ultra performance liquid chromatography-tandem mass spectrometry （UPLC/MS/MS） and magnetic multiwalled carbon nanotubes cleaning. The samples were extracted with acetonitrile and cleaned up by magnetic multiwalled carbon nanotubes. The target analytes were separated by Waters CORTECSTM C18 ＋ column with gradient elution using methanol and 0. 1% formate in water as mobile phases. The analytes were detected by tandem quadrupole mass spectrometry after positive electrospray ionization by multiple reaction monitoring （MRM）. External standard method with matrix was used to determine the results. The correlation coefficient was greater than 0.99 for each pesticide. The limits of quantitation （LOQs） were 0. 3 - 3.0 μg/kg. The mean recoveries at the three spiked levels of 5.0, 25.0, 50.0 μg/kg were 80. 1% - 102. 3%, respectively. The relative standard deviations （RSDs） were 1.9% -9.4%. The results indicated that using magnetic muhiwalled carbon nanotubes as adsorbent was efficient for the purification. The simplicity, sensitivity and good precision of the method made it suitable for determination of pesticide residues in vegetables.

关 键 词：磁性多壁碳纳米管 超高效液相色谱-串联质谱 农药 残留 

分 类 号：O657.63[理学—分析化学]