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首页> 外文学位 >Multiresidue determination of pesticides in fruits and vegetables by liquid chromatography tandem mass spectrometry with on-line sample clean-up technique.
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Multiresidue determination of pesticides in fruits and vegetables by liquid chromatography tandem mass spectrometry with on-line sample clean-up technique.

机译：液相色谱-串联质谱-在线样品净化技术对水果和蔬菜中的农药进行多残留测定。

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摘要

A novel on-line sample clean-up and trace enrichment technique was developed for determination of pesticides in fruits and vegetables utilizing liquid chromatography tandem mass spectrometry. This technique uses an on-line solid phase extraction cartridge and column-switching device to reduce tedious off-line wet chemistry operations. The efficiency and recovery of sample preparation is significantly improved.;One hundred and five pesticides with a wide variety of chemical properties are included in the method development of determination of multiresidue pesticides in apple, cucumber, spinach, and tomato. A universal reversed phase high performance liquid chromatography method was used as a separation technique. An Atmospheric Pressure Chemical Ionization (APCI) interface coupled to a triple quadrupole mass spectrometer was employed for detection and quantitation. The ionization mechanisms of the pesticides with different chemical properties in the APCI ion source are discussed. A sensitive multiresidue pesticide screening method using selective ion monitoring (SIM) and selective reaction monitoring techniques (SRM) in both positive and negative modes, was developed. Out of the 105 pesticides studied, 98 in apple, 98 in cucumber, 84 in spinach and 98 in tomato have limits of detection of 10 parts per billion (ppb) or better. All carbamates, organophosphorus and triazines have limits of detection less than 10 ppb. Those pesticides that have high limits of detection are mostly multiple chlorine-containing pesticides, especially chlorinated hydrocarbons. The variables of mass spectrometry that determine the detection sensitivity of pesticides are also discussed. The recovery studies were carried out three times. The average recoveries are 94.7%, 96.6%, 91.8%, and 93.8% for apple, cucumber, spinach, and tomato, respectively. The average relative standard deviations (RSD) of triplicate recovery studies is 5.6% between 1.8% and 12.1%.;Two new concepts of mass spectrometry data acquisition, dynamic selective ion monitoring (DSIM) and dynamic selective reaction monitoring (DSRM) techniques, were created. This is an instrument control computer program designed exclusively on the Finnigan TSQ 7000 system. DSIM and DSRM are techniques which can tolerate retention time drift from run to run without missing pesticide peaks, which often happens in conventional SIM and SRM technique when retention times of peaks shift considerably.
机译：开发了一种新颖的在线样品净化和痕量富集技术，用于利用液相色谱串联质谱法测定水果和蔬菜中的农药。该技术使用在线固相萃取滤芯和色谱柱切换装置来减少繁琐的离线湿法化学操作。苹果样品，黄瓜，菠菜和番茄中多残留农药的测定方法开发中包括了105种具有多种化学特性的农药。采用通用的反相高效液相色谱法作为分离技术。使用与三重四极杆质谱仪耦合的大气压化学电离（APCI）接口进行检测和定量。探讨了化学性质不同的农药在APCI离子源中的电离机理。开发了一种灵敏的多残留农药筛查方法，该方法使用正离子和负离子两种方式使用选择性离子监测（SIM）和选择性反应监测技术（SRM）。在所研究的105种农药中，苹果中的98种，黄瓜中的98种，菠菜中的84种和番茄中的98种农药的检出限为十亿分之10（ppb）或更高。所有氨基甲酸酯，有机磷和三嗪的检出限均低于10 ppb。具有高检测限的那些农药大多是多种含氯农药，尤其是氯代烃。还讨论了确定农药检测灵敏度的质谱变量。恢复研究进行了三次。苹果，黄瓜，菠菜和番茄的平均回收率分别为94.7％，96.6％，91.8％和93.8％。一式三份回收率研究的平均相对标准偏差（RSD）为5.6％，介于1.8％和12.1％之间。质谱数据采集的两个新概念分别是动态选择性离子监测（DSIM）和动态选择性反应监测（DSRM）技术。创建。这是专门在Finnigan TSQ 7000系统上设计的仪器控制计算机程序。 DSIM和DSRM是可以容忍每次运行之间保留时间漂移而不会丢失农药峰的技术，这在传统的SIM和SRM技术中通常会在峰的保留时间发生明显变化时发生。

著录项

  • 作者

    Yu, Xiao.;

  • 作者单位

    Rutgers The State University of New Jersey - New Brunswick.;

  • 授予单位 Rutgers The State University of New Jersey - New Brunswick.;
  • 学科 Agriculture Food Science and Technology.;Environmental Sciences.;Chemistry Analytical.
  • 学位 Ph.D.
  • 年度 2000
  • 页码 106 p.
  • 总页数 106
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

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