QuEChERS结合高效液相色谱串联质谱快速检测速溶茶粉中八种农药残留

Rapid determination of 8 pesticide residues in instant tea power by QuEChERS-HPLC-MS/MS

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MgSO_4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(R^2)在0.996 9~0.999 8,定量限(LOQs)为0.2~1μg/kg,平均加标回收率为61%~118%。建立的QuEChERS-HPLCMS/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 Qu EChERS 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（ R^2） 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.