色谱2017，Vol.35Issue(9)：941-948,8.DOI:10.3724/SP.J.1123.2017.06001
超高效液相色谱-四极杆-飞行时间质谱法快速筛查姜和葱中44种农药残留
Rapid screening of 44 pesticide residues in ginger and scallion by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry
摘要
Abstract
An analytical method was established for the simultaneous determination of 44 pesti-cide residues in ginger and scallion by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry ( UPLC-Q-TOF/MS) . The samples were extracted with acetonitrile containing 0. 1% ( v/v) acetic acid aqueous solution, and cleaned-up by primary secondary amine ( PSA) and octadecyl bonded silica ( C18 ) adsorbents. The compounds were separated on a Poroshell 120 SB-C18 column (100 mm×3. 0 mm, 2. 7μm) with 0. 1% (v/v) for-mic acid aqueous solution containing 5 mmol/L ammonium acetate-acetonitrile as mobile pha-ses under gradient elution. The eluent was determined by UPLC-Q-TOF/MS with electrospray ionization in positive mode. The quantification analysis was performed with the external stand-ard method. In all ions MS/MS mode, the compounds were qualitatively screened and con-firmed by one data acquisition. The correlation coefficients ( r) were greater than 0. 995 in the linear ranges of the 44 pesticides. The limits of quantification ( LOQs, S/N=10) of the 44 pesti-cides were 2. 5-5. 0 μg/kg. At the three spiked levels, the recoveries were between 73. 4% and 113. 7% with the relative standard deviations ( RSDs) ranging from 0. 7% to 12. 1% ( n=6) . The method effectively improves the determination efficiency of pesticide residues screening by high-resolution mass spectrometry.关键词
超高效液相色谱-四极杆-飞行时间质谱/高分辨全离子二极质谱技术/QuEChERS/筛查/农药残留Key words
ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry ( UPLC-Q-TOF/MS )/high-resolution all ions MS/MS technology/QuECh-ERS/screening/pesticide residues分类
化学化工引用本文复制引用
刘永强,刘胜,许文娟,田国宁,张金玲..超高效液相色谱-四极杆-飞行时间质谱法快速筛查姜和葱中44种农药残留[J].色谱,2017,35(9):941-948,8.基金项目
山东出入境检验检疫局科研课题(SK201613) （SK201613）
国家质检总局科技计划项目(2016IK202).Program of Shandong Entry-Exit Inspection&Quarantine Bureau (No.SK201613) （2016IK202）
Science and Technology Project of Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China (No.2016IK202) . （No.2016IK202）
