超高效液相色谱-串联质谱法测定猪肝中有机磷农药残留量的研究  

Determination of Organophosphorus Pesticide Residues in Pig Liver by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：刘琪[1] 孙雷[1] 张骊[1] 

机构地区：[1]中国兽医药品监察所,北京100081

出　　处：《分析测试学报》2010年第7期747-750,共4页Journal of Instrumental Analysis

基　　金：国家科技支撑计划课题资助项目(2006BAD31B09)

摘　　要：建立了猪肝组织中敌百虫、敌敌畏、马拉硫磷、巴胺磷、倍硫磷、二嗪农和辛硫磷7种有机磷农药残留的超高效液相色谱-串联质谱（UPLC-MS/MS）测定方法。样品经乙酸乙酯提取后,用Carb/PSA（碳黑/乙二胺-N-丙基）复合萃取柱净化,经超高效液相色谱仪和C18色谱柱分离,以甲醇和10 mmol/L乙酸铵水溶液为流动相进行梯度洗脱。电喷雾正离子模式（ESI＋）电离,多反应监测模式（MRM）检测,外标法定量。结果表明：7种有机磷农药标准溶液在10~1 000μg/L范围内呈现良好的线性关系,r2均不小于0.995 0,方法检出限为5μg/kg,定量下限为10μg/kg;7种有机磷农药在10~50μg/kg添加水平范围内的回收率为70%~92%,批内、批间RSD均小于16%。该方法具有简便、快捷、灵敏度高、定性准确等优点,满足食品安全检测有关法规的要求。An ultra performance liquid chromatography-tandem mass spectrometric（UPLC-MS/MS） method was developed for the simultaneous determination of trichlorphon,dichlorvos,malathion,propetamphos,fenthion,diazinon,phoxim residues in pig liver.The samples were extracted by ethyl acetate,and cleaned up with PSA/Carb solid phase extraction（SPE） column.The separation of organophosphorus pesticides was performed on a C18 column（50 mm×2.1 mm,1.7 μm） with gradient elution solvent of methanol（A） and 10 mmol/L ammonium acetate（B） at a flow rate of 0.35 mL/min.The electrospray was operated in the positive ionization mode and 7 organophosphorus pesticides were identified under multiple reaction monitoring（MRM） mode.The method was quantified by external standard method.The calibration curves were in good linearity between the peak area and the concentration of 10-1 000 μg/L for 7 organophosphorus pesticides with correlation coefficients r20.995 0.The detection limits of 7 organophosphorus pesticides were 5 μg/kg,and the quantification limits were 10 μg/kg.The average recoveries from animal tissues spiked at concentration range of 10-50 μg/kg ranged from 70% to 92%.The relative standard deviations of intra-and inter-batch were both less than 16%.

关 键 词：超高效液相色谱-串联质谱 有机磷农药 残留 猪肝 

分 类 号：O657.72[理学—分析化学] F767.2[理学—化学]