超高效液相色谱-四极杆飞行时间质谱法非靶向快速筛查进口粮谷中未知的农药残留

Rapid screening of pesticide residues in imported grains by ultra-performance liquid chromatography-quadrupole-time of flight mass spectrometry

利用快速提取农药(fast pesticide extraction,FaPEx)方法前处理样品,并结合超高效液相色谱-四极杆飞行时间质谱(UPLC-Q-TOF)技术建立了非靶向快速筛查进口粮谷中未知的多种农药残留方法。采用1%(v/v)醋酸乙腈溶液提取粮谷中未知的农药残留,FaPEx固相萃取柱净化、浓缩,UPLC-Q-TOF检测。利用目标化合物特征离子的精确质量数、同位素匹配、二级碎片信息和保留时间进行数据库匹配,筛查可疑未知农药。结果表明,该方法无需对照标准品即可快速筛查进口粮谷中的农药残留,能够应用于进口粮谷样品的实际筛查。该方法快速、准确、分析通量高,可以为进口粮谷中农药残留的快速筛查和质量控制提供重要的方法依据。

A fast sample pretreatment method by fast pesticide extraction （FaPEx） method combined with ultra-performance liquid chromatography-quadrupole-time of flight mass spec-trometry was developed for screening of unknown pesticide residues in imported grains. The samples were extracted with 1% （v / v ） acetic acid acetonitrile solution,cleaned-up by solid phase extraction column with FaPEx cartridges,and determined by UPLC-Q-TOF. The data was compared with the library with the accurate mass,isotopic distribution,fragmentation information and retention time. The results showed that this method can be used for the rapid screening of pesticide residues in imported grains without the reference standards, and it was applied to the actual screening of imported grain samples. The method is high efficiency, sensi-tivity and accuracy, which can meet the requirement for the rapid screening of pesticide resi-dues in imported grains.