高效液相色谱-串联质谱法快速测定果蔬中特丁硫磷、特丁硫磷砜和特丁硫磷亚砜的残留量  

Rapid determination of terbufos, terbufos-sulfone and terbufos-sulfoxide residues in vegetables and fruits by high performance liquid chromatography-tandem mass spectrometry

作　　者：刘佳 蔡涛 庞宏宇[1] 罗华兰[1] 王震[1] 李俊[1] 赖飞[1] 杜楠[1] 丁静 王晓鹭 周雪丽[1] 祝愿 LIU Jia;CAI Tao;PANG Hong-Yu;LUO Hua-Lan;WANG Zhen;LI Jun;LAI Fei;DU Nan;DING Jing;WANG Xiao-Lu;ZHOU Xue-Li;ZHU Yuan(Guizhou Agricultural Products Quality and Safety Supervision and Testing Center,Guiyang 550001,China)

机构地区：[1]贵州省农产品质量安全监督检验测试中心,贵阳550001

出　　处：《食品安全质量检测学报》2019年第2期476-481,共6页Journal of Food Safety and Quality

基　　金：贵州省重大科技专项项目(黔科合重大专项字[2013]6024号)~~

摘　　要：目的建立高效液相色谱-串联质谱法快速测定蔬菜、水果中特丁硫磷、特丁硫磷砜和特丁硫磷亚砜农药残留量的分析方法。方法样品经乙腈直接匀浆提取过滤,滤液中加入氯化钠分层后吸取上层清液过0.22μm滤膜,经Phenomenex C_(18)(150 mm×2.0 mm, 5μm)色谱柱,以0.1%乙酸铵甲醇溶液和0.1%甲酸乙酸铵水溶液为流动相,梯度洗脱,流速为0.5mL/min,柱温为35℃,多重态反应监测模式监测。结果在14.4～288μg/L的浓度范围内,各组分线性关系良好(r>0.999),检出限为0.12～0.63μg/kg,加标回收率为84.8%～103.0%,相对标准偏差为0.473%～15.622%。结论该方法分析速度快、灵敏度高,适合于蔬菜、水果中特丁硫磷类残留物的检测。Objective To establish a method for rapid determination of terbufos,terbufos-sulfone and terbufos-sulfoxide residues in vegetables and fruits by high performance liquid chromatography-tandem mass spectrometry.Methods The samples were extracted and filtered with acetonitrile homogenate,sodium chloride was added to the filtrate and the filtrate was filtered by0.22 microns filter membrane after the supernatant was absorbed.The samples were separated with a Phenomenex C18(150 mm×2.0 mm,5 μm)colum using 0.1% ammonium acetate in methanol and 0.1% ammonium formate acetate as mobile phase at the flow of 0.5 mL/min by gradient elute,and the column temperature was maintained at 35 ℃.The detection was monitored by multiple reaction monitoring.Results At the concentration range of 14.4-288 μg/L,the linear relationship of the components was good(r>0.999),the limits of detection were 0.12-0.63 μg/kg,the standard recoveries were 84.8%-103.0%,and the relative standard deviations were 0.473%-15.622%.Conclusion This method has the advantages of high speed analysis and high sensitivity,and is suitable for detecting terbutazone residues in vegetables and fruits.

关 键 词：特丁硫磷 特丁硫磷砜 特丁硫磷亚砜 高效液相色谱-串联质谱法 蔬菜水果 

分 类 号：O657.63[理学—分析化学] TS207.3[理学—化学]