利用QuEChERS结合高效液相色谱串联质谱(HPLC-MS/MS)建立了速溶茶粉中8种农药残留(克百威、内吸磷、灭线磷、甲胺磷、辛硫磷、吡蚜酮、硫环磷、氯唑磷)的检测方法。样品经水-乙腈提取,无水MgSO4和N-丙基乙二胺(PSA)净化后,采用高灵敏度的HPLC-MS/MS检测,优化HPLC-MS/MS条件使8种农药在10 min内完成色谱分离,基质匹配外标法定量。各种农药在添加水平范围内均有良好的线性关系,相关系数(R2)在0.996 9~0.999 8,定量限(LOQs)为0.2~1 μg/kg,平均加标回收率为61%~118%。建立的QuEChERS-HPLC-MS/MS方法简单、快速、灵敏度高、准确度高,可以满足对速溶茶粉中多种农药残留同时检测的要求。
A method was established for the determination of 8 pesticide residues (carbofuran, demeton(o+s), ethoprophos, methamidophos, phoxim, pymetrozine, phosfolan, isozofos) in instant tea powde r on the basis of QuEChERS combined with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).The sample was extracted by water-acetonitrile and cleaned by magnesium sulfate anhydrous and PSA, and then determined by the highly sensitive HPLC-MS/MS.The HPLC-MS/MS conditions were optimized to complete chromatographic separation of 8 pesticide residues within 10 minutes.The pesticide residues were quantified by matrix-matched external standard method.The calibration curves of different samples showed good linearity within the concentrations of spiked levels, the correlation coefficients (R2) were 0.996 9-0.999 8, the limits of quantification (LOQs) were 0.2-1 μg/kg, and the average recoveries were 61%-118%.The QuEChERS-HPLC-MS/MS method was simple, rapid, sensitive, accurate and was applicable for the determination of multiple pesticide residues in instant tea power simultaneously.