高效液相色谱-四极杆-飞行时间质谱法快速筛查蔬菜中124种药物与个人护理品残留量

Rapid screening of 124 kinds of pharmaceuticals and personal care products in vegetables by high performance liquid chromatography quadrupole time of flight mass spectrometry

目的基于高效液相色谱-四极杆-飞行时间质谱法(high performance liquid chromatography quadrupole time of flight mass spectrometry,LC-QTOF/MS)建立蔬菜中124种药物和个人护理品(pharmaceuticals and personal care products,PPCPs)的同时快速筛查、确证和定量分析方法。方法样品经过10 m L乙腈提取,改进QuEChERS方法净化,电喷雾电离模式,外标法定量;建立一级精确质量数据库、色谱保留时间和二级质谱库,实现蔬菜中124种目标污染物的快速筛查和确证。结果在5~500μg/L质量浓度范围内,124种目标化合物的线性关系良好(r>0.99)。多种蔬菜基质中10、50、200μg/kg的3个加标水平下平均回收率为62.7%~117.2%,相对标准偏差为1.6%~8.9%。满足痕量分析要求,基质干扰效应消除效果较好,该方法具有良好的净化效果。结论该方法具有操作简便;耗时短;灵敏度高;稳定性好的优点,适用于蔬菜基质中PPCPs的筛查检测及定量分析,对蔬菜质量安全的快速筛查具有技术支撑意义。

Objective To establish a method for simultaneous screening,confirmation and quantitative analysis of 124 kinds of pharmaceuticals and personal care products(PPCPs)in vegetables based on high performance liquid chromatogre-quadrupole time-of-flight mass spectrometry(LC-QTOF/MS).Methods The samples were extracted by 10 mL acetonitrile,purified by QuEChERS method,electrospray ionization mode,and quantified by external standard method.The primary accurate mass database,chromatographic retention time and secondary mass spectrometry database were established to realize the rapid screening and confirmation of 124 kinds of target pollutants in vegetables.Results In the mass concentration range of 5–500μg/L,the linear relationship of 124kinds of compounds was good(r>0.99).The average recoveries at 10,50 and 200μg/kg were 62.7%–117.2%,and the relative standard deviations were 1.6%–8.9%.The method meets the requirements of trace analysis and eliminates the interference of vegetable matrix.Conclusion The method is simple,time-saving,sensitive and stable,which is suitable for the screening and quantitative analysis of PPCPs in vegetables.