非靶向快速筛查茶饮料中未知农药残留

本文建立了分散液液微萃取-高效液相色谱-四极杆-飞行时间质谱法(DLLME/HPLC-Q-TOF/MS)非靶向快速筛查茶饮料中未知农药残留的方法。根据目标化合物特征离子的精确质量数、同位素匹配、二级碎片信息进行数据库匹配,筛查可疑未知农药。依据13种农药为质控化合物优化了测定方法。结果表明,2 g N-丙基乙二胺为预净化剂,甲醇为分散剂,200 μL三氯甲烷为萃取剂,通过摇床震荡的方式提取茶饮料中的目标化合物,Xbridge BEH C18色谱柱分离的方法回收率范围为83.1%~96.8%,RSD范围在0.88%~4.82%。空白基质校准曲线的线性范围为2~400 μg/L,决定系数R2在0.9989以上,检测限为0.002~0.092 μg/kg,定量限为0.006~0.307 μg/kg。该方法无需标准品即可快速筛查茶饮料中的农药残留,能够应用于茶饮料样品的实际筛查。该方法快速、准确、分析通量高,可以为茶饮料中农药残留的快速筛查和质量控制提供重要的方法依据。

Non-target Rapid Screening of Unknown Pesticide Residues in Tea Beverage

A dispersive liquid-liquid microextraction(DLLME)coupled with high performance liquid chromatography-quadrupole-time of flight mass spectrometry(HPLC-Q-TOF/MS)method was developed for screening of unknown pesticide residues in tea beverage. 13 kinds of quality-controlled compounds were used as indicator to optimize this method. The target compounds in samples were cleaned by 2 g PSA,extracted by 200 μL trichloromethane and dispersed by methanol in shaking table and separated on a C18 column,and determined by HPLC-Q-TOF/MS.The average recoveries were between 83.1%~96.8%,and RSD ranged from 0.88%~4.82%.The matrix calibration curves showed good linearity in the range of 2.0~400 μg/L,the coefficient of determination was above 0.9989,the limits of detection(LOD,S/N=3)was 0.002~0.092 μg/kg,and the limits of quatitation(LOQ,S/N=10)was 0.006~0.307 μg/kg. This method can quickly screen pesticide residues in tea beverage without reference standards,and can be applied to the actual screening of tea beverage samples. This method is fast,accurate and has high throughput,which can meet the requirement for non-target rapid screening of pesticide residues in tea beverage.