【摘要】 目的建立蔬菜中8种杀虫剂(涕灭威、克百威、涕灭威亚砜、涕灭威砜、3-羟基克百威、吡虫啉、啶虫脒、氯虫苯甲酰胺)残留量的超高效液相色谱-串联质谱测定方法。方法样品经乙腈提取、Qu ECh ERS净化,采用CORTECS UPLC C18柱(100 mm×2.1 mm,1.6μm)分离,以0.1%甲酸水溶液和含0.1%甲酸的乙腈为流动相进行梯度洗脱,正离子模式下多反应监测(MRM)方式检测,外标法定量。结果 8种杀虫剂的线性范围为0.5 ng/ml~200 ng/ml,相关系数均>0.999。检出限为0.10μg/kg~0.52μg/kg,定量限为0.30μg/kg~1.56μg/kg;在加标水平为0.02 mg/kg、0.1 mg/kg、0.4 mg/kg时,平均加标回收率为87.8%~108%,相对标准偏差(RSD)在2.2%~9.0%。62份蔬菜样品中检出涕灭威亚砜1份,3-羟基克百威5份,克百威3份,吡虫啉6份,啶虫脒5份,氯虫苯甲酰胺1份,涕灭威砜及涕灭威未检出。结论该方法简便、灵敏、准确,符合分析要求,适合蔬菜中8种杀虫剂残留量检测的要求。更多还原

【Abstract】 Objective To establish a method of ultra-high performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS) for detecting 8 insecticides( aldicarb,carbofuran,aldicarb sulfoxide,aldicarb sulfone,3-hydroxy carbofuran,imidacloprid,acetamiprid,chlorantraniliprole) in vegetables. Methods The samples were extracted with acetonitrile and cleaned-up by Qu ECh ERS method. 8 insecticides were separated on a CORTECS UPLC C18 column( 100 mm × 2. 1 mm,1. 6 μm) with the gradient elution using the mobile phases of acetonitrile containing 0. 1% formic acid and water containing0. 1% formic acid. The analytes were detected in a positive ion multiple reaction mode( MRM) using external standard method.Results The liner ranges of 8 insecticides were 0. 5 ng/ml-200 ng/ml,with the correlative coefficients greater than 0. 999.The limits of detection( LOD) was within 0. 10 μg/kg-0. 52 μg/kg,the limits of quantification( LOQ) was within 0. 30 μg/kg-1. 56 μg/kg. When the standard levels were respectively at 0. 02 mg/kg,0. 1 mg/kg,0. 4 mg/kg,the recoveries of the method ranged from 87. 8% to 108%,and the relative standard deviations( RSDs) ranged from 2. 2% to 9. 0%. Aldicarb sulfoxide was detected in 2 samples,3-hydroxy carbofuran in 5 sample,carbofuran in 3 samples,imidacloprid in 6 samples,acetamipridin6 sample,chlorantraniliprole in 1 sample,but aldicarb and aldicarb sulfone were not detected in the rest samples. Conclusion This method is simple,sensitive,accurate and it is suitable for the determination of 8 insecticides in vegetables.更多还原