牛肉中7种拟除虫菊酯类农药残留的固相萃取-超高效液相色谱-串联质谱法测定  

Simultaneous Determination of 7 Pyrethroids Pesticide Residues in Cattle Muscle by SPE-UPLC-MS/MS

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10期1048-1052,共5页Journal of Instrumental Analysis

基　　金：国家科技支撑计划课题资助项目(2006BAD31B09)

摘　　要：建立了牛肉组织中胺菊酯、氯氰菊酯、溴氰菊酯、氟胺氰菊酯、氰戊菊酯、氟氯苯氰菊酯、氯菊酯7种拟除虫菊酯类农药残留的超高效液相色谱-串联质谱测定方法,样品经乙腈提取后,吹干提取液,用正己烷溶解,氟罗里硅土固相萃取柱净化,经BEHC18色谱柱分离,以0.1%甲酸的甲醇溶液和0.1%乙酸铵溶液为流动相进行洗脱。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种拟除虫菊酯类农药标准溶液在10～1000μg/L范围内呈良好线性,r2均大于0.998;方法检出限为5μg/kg,定量下限为10μg/kg;7种拟除虫菊酯农药在10～50μg/kg添加水平内的回收率为81%～116%,批内、批间RSD均小于15%。该方法具有简便快捷、灵敏度高、定性准确等优点,能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 established for the simultaneous determination of tetramethrin,cypermethrin,deltamethrin,fluvalinate,fenvalerate,flumethrin,permethrin residues in cattle muscle.The samples were extracted by acetonitril,cleaned up with Florisil PR solid phase extraction（SPE）column.The separation of pyrethroids pesticide was performed on Waters Acquity UPLC-Premier XE system with BEH C18 column（50 mm×2.1 mm,1.7 μm）and the elution solvent of methanol（containing 0.1% formic acid）and water（containing 0.1% ammonium acetate）at a flow rate of 0.3 mL/min.The electrospray was operated under the positive ionization mode and 7 pyrethroids pesticides were identified under multiple reaction monitoring（MRM）mode.The method was quantified by the external standard method.The calibration curves were linear between the peak areas and the concentrations in the range of 10-1 000 μg/L with correlation coefficients（r2）more than 0.998.The limit of detection for 7 pyrethroids pesticides were all 5 μg/kg,and the limit of quantitation were 10 μg/kg.The average recoveries for the spiked cattle tissues at three concentrations of 10-50 μg/kg ranged from 81% to 116% and the relative standard deviations for intra-and inter-batch were both less than 15%.The proposed method was easy,sensitive,accurate and could meet the requirements for food safety detection.

关 键 词：固相萃取 超高效液相色谱-串联质谱 拟除虫菊酯 残留 牛肉 

分 类 号：O657.63[理学—分析化学] F767.2[理学—化学]