Rapid Screening and Determination of 248 Pesticide Residues in Apples and Lettuces by Liquid Chromatography-Quadrupole Time-of-flight Mass Spectrometry
Rapid Screening and Determination of 248 Pesticide Residues in Apples and Lettuces by Liquid Chromatography-Quadrupole Time-of-flight Mass Spectrometry[J]. 2018,37(2):154-164.
Rapid Screening and Determination of 248 Pesticide Residues in Apples and Lettuces by Liquid Chromatography-Quadrupole Time-of-flight Mass Spectrometry[J]. 2018,37(2):154-164.DOI:
基于液相色谱-四极杆-飞行时间质谱(LC-QTOF/MS)建立了苹果和生菜中248种农药残留的同时快速筛查、确证和定量分析方法。样品经10 mL乙腈和5 mL 0.1%乙酸水溶液提取,改进QuEChERS法净化,电喷雾电离,正离子扫描,SWATH-MS扫描模式检测,基质匹配外标法定量;建立了一级精确质量数据库、色谱保留时间和二级质谱库,实现了苹果、生菜中248种目标农药的快速筛查和确证。在0.010~0.200 mg/L 质量浓度范围内,248种目标化合物的线性关系良好(r>099)。248种农药的定量下限均为0.010 mg/kg。苹果、生菜中0.010、0.050、0.100 mg/kg 3个加标水平下的平均回收率分别为25.2%~128%,32.4%~132%和28.9%~133%,相对标准偏差(RSD)为0.98%~21.2%。该方法操作简便、耗时短、灵敏度高、稳定性好,适用于苹果和生菜中农药残留的筛查检测及定量分析,可显著降低检测成本,具有实际应用价值。
Abstract
A method for the simultaneous screening and determination of 248 pesticide residues in apples and lettuces was developed by liquid chromatography coupled with high resolution quadrupole time-of-flight mass spectrometry(LC-Q TOF/MS).The samples were extracted with 10 mL acetonitrile and 5 mL 0.1%(by volume) acetic acid,cleaned up by a modified QuEChERS method.Confirmation was achieved by electro-spray ionization(ESI) in positive mode using SWATH MS acquisition,and quantification was carried out by external standard method.Two databases of accurate mass and fragment ions were created.The standard matrix-matched calibration curves of 248 target compounds were linear in the range of 0.010-0.200 mg/L,with the correlation coefficients(r) larger than 0.99.The limits of quantification for 248 target compounds all were 0.010 mg/kg.The mean recoveries for the target compounds at three spiked levels of 0.010,0.050,0.100 mg/kg ranged from 25.2% to 128%,32.4% to 132%and 28.9% to 133%,respectively with relative standard deviations of 0.98%-21.2%(n=6).With the advantages of simplicity,timesaving,high sensitivity and good stability,the method was applicable for the simultaneous screening and determination of 248 pesticide residues in apples and lettuces,and could significantly reduce the test cost.
关键词
液相色谱-四极杆飞行时间质谱高分辨质谱农药残留筛查苹果生菜
Keywords
LC-Q TOF/MShigh resolution mass spectrometrypesticide residuesscreeningapplelettuces