固相萃取-液相色谱-串联质谱法测定水果和土壤中四螨嗪残留量  

Determination of clofentezine in four fruits and soil by SPE-liquid chromatography-triple quadrupole tandem mass spectrometry

作　　者：张志勇 单炜力[2] 简秋[2] 沈燕 刘贤金 

机构地区：[1]江苏省食品质量安全重点实验室/农业部食品安全监控重点开放实验室,南京210014 [2]农业部农药检定所,北京100125

出　　处：《分析试验室》2013年第1期35-38,共4页Chinese Journal of Analysis Laboratory

基　　金：江苏省农业科技自主创新资金项目(CX(11)2072)资助

摘　　要：建立了水果和土壤样品中四螨嗪的液相色谱-电喷雾串联质谱检测方法。水果或土壤样品用丙酮提取,经弗罗里硅土柱净化,以Agilent ZORBAX SB-C18色谱柱分离,以电喷雾电离串联质谱正离子多反应监测模式进行测定。对四螨嗪在水果和土壤中在4个不同添加水平下的回收率进行了测定,结果表明,四螨嗪在柑橘(全果)中的添加回收率为86.9%～93.1%(RSD为7.4%～9.4%),在苹果中的添加回收率为84.1%～95.1%(RSD为5.9%～9.7%),在葡萄中的添加回收率为88.8%～93.7%(RSD为8.0%～10.1%),在梨中的添加回收率为88.6%～96.1%(RSD为7.0%～10.2%),在土壤中的添加回收率为83.0%～96.8%(RSD 6.7%～12%)。该方法满足农药残留检测要求,适用于水果和土壤中四螨嗪残留的检测。A method was developed for the determination of clofentezine residues in four fruits and soil by using liquid chromatography coupled with electrospray ionization tandem mass spectrometry（LC-ESI-MS/MS）.The residues of clofentezine in fruits and soil samples were extracted by acetone and cleaned up by Florisil column method,and then analyzed by using LC-MS/MS in multiple reaction monitoring（MRM） mode via positive electrospray ionization with an Agilent ZORBAX SB-C18 as the analytical column.The method was validated at four of fortification levels in fruits and soil.The validation results were as follows： the recoveries of clofentezine in citrus（whole） were from 86.9% to 93.1%（RSD： 7.4% - 9.4%）,in apple were from 84.1% to 95.1%（RSD： 5.9% - 9.7%）,in grape were from 88.8% to 93.7%（RSD： 8.0% - 10.1%）,in pear were from 88.6% to 96.1%（RSD： 7.0% - 11%）,in soil were from 83.0% to 96.8%（RSD： 6.7% - 12%）.The results show that the method is simple,rapid and characterized with acceptable sensitivity and accuracy to meet the requirements of the pesticide residue analysis.This method is applicable to confirm the residues of clofentezine in fruits and soil.

关 键 词：固相萃取 液相色谱-串联质谱 四螨嗪 水果 残留 

分 类 号：O657.63[理学—分析化学]