多壁碳纳米管作为吸附剂的QuEChERS-气相色谱-四极杆飞行时间质谱快速筛查淡水产品中145种农药残留

Rapid Screening of 145 Pesticide Residues in Limnetic Products by Gas Chromatography-Quadrupole Time of Flight Mass Spectrometry and QuEChERS with Multi-walled Carbon Nanotubes

建立了基于多壁碳纳米管（MWCNTs）的新型Qu ECh ERS前处理方法,结合气相色谱-高分辨飞行时间质谱对淡水产品中145种农药残留进行快速筛查。样品采用水和乙腈提取,以MWCNTs为净化吸附剂,用Qu ECh ERS方法处理后,采用气相色谱-四极杆飞行时间质谱（GC-QTOF/MS）检测,外标法定量。研究并优化了提取条件、吸附剂种类及用量、GC-QTOF/MS采集速率及质量提取窗口。在最佳实验条件下,145种农药在5-200μg/kg范围内线性关系良好（r2〉0.98）,10,20,100μg/kg 3个添加水平下的回收率为69.4%-114.2%,相对标准偏差（RSD,n=6）为2.2%-13.8%,定量下限为1.1-40.0μg/kg。与传统Qu ECh ERS方法相比,所建立的方法快速、准确,净化效果明显,可显著降低基质干扰。

A modified QuEChERS（ quick, easy, cheap, effective, rugged, safe） method based on multi-walled carbon nanotubes（MWCNTs） was established for the simultaneous determination of 145 pesticide residues in limnetic products by gas chromatography- quadrupole time of flight mass spec- trometry（ GC -QTOF/MS）. The samples were extracted with water and acetonitrile, purified by QuEChERS with MWCNTs, determined by GC -QTOF/MS. The quantification analysis was per- formed with the external standard calibration. The extraction conditions, type and amount of adsor- bents, acquisition rate and extraction window of GC - QTOF/MS were optimized. Under the optimal conditions, the results indicated that the calibration curves were linear （ r2 〉 0. 98 ） in the range of 5 -200 μg/kg. The recoveries for 145 pesticides were in the range of 69.4% -114.2% at three spiked levels of 10, 20, 100 μg/kg, with relative standard deviations （ RSD, n = 6 ） of 2.2% -13.8%. The limits of quantitation were in the range of 1.1 -40.0 μg/kg. Compared to the original QuEChERS method, the proposed method was rapid and accurate, and could significantly reduce matrix interference.