摘要
建立了采用固相萃取-超高效液相色谱-质谱/质谱法(SPE-LC-MS/MS)对叶菜中11种氨基甲酸酯农药(克百威、3羟基克百威、甲萘威、仲丁威、异丙威、抗牙威、速灭威、灭多威、涕灭威、涕灭威亚砜、涕灭威砜)残留同时测定的方法。样品用乙腈提取后经氨基固相萃取柱净化处理,经Acquity UPLCTM BEH C18(100 mm×2.1 mm,1.7μm)色谱柱分离后测定,该方法采用多反应监测(MRM)离子扫描模式,外标法进行定量,线性良好(r2>0.994),检出限为0.001～0.004 mg/kg,总体回收率为80.4%～99.8%,相对标准偏差为3.4%～10.8%。该方法的定量限满足目前国内外药物的最大残留限量要求,可作为叶菜中相关药物残留的筛选检测方法。
Residual amounts of 11 carbamate were determined by UPLC-MS/MS.The sample was extracted with acetonitrile and extract was purified on NH2 SPE column.The eluate was separated by gradient elution with methanol,formic acid and water solution of different ratio on Acquity UPLCTM BEH C18（100 mm×2.1 mm,1.7 μm） column and determined by LC-MS/MS,using positive-ion electrospray ionization in multiple reaction monitoring（MRM） mode.External standard method was used to determine the residue contents with a good linear relationship（r20.994）.The limits of quantification（LOQ） was 0.001 mg/kg～0.004 mg/kg.The recovery ranges were from 80.4% to 99.8% with the relative standard deviations（RSDs） between 3.4% and 10.8%.As a screening method,the developed procedure is suitable for the determination and confirmation of the drug residues in leafy vegetables samples.
出处
《热带农业科学》
2012年第3期69-73,共5页
Chinese Journal of Tropical Agriculture
