Canadian Food Inspection Agency Calgary Laboratory, 3650 36th Street NW, Calgary, Alberta, Canada.
J Agric Food Chem. 2010 May 26;58(10):5904-25. doi: 10.1021/jf902747t.
Applications of liquid chromatography electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) and ultrahigh-pressure liquid chromatography electrospray ionization quadrupole time-of-flight mass spectrometry (UHPLC QqTOF MS) for the determination of 148 pesticides in berry fruits are presented in this study. Pesticides were extracted from berries using a procedure known as QuEChERS (quick, easy, cheap, effective, rugged, and safe). Quantification, with an analytical range from 5 to 500 microg/kg, was achieved using matrix-matched standard calibration curves with isotopically labeled standards or a chemical analogue as internal standards. The method performance parameters, which included overall recovery, intermediate precision, and measurement uncertainty, were evaluated according to a designed experiment, that is, the nested design. For LC/ESI-MS/MS, 95% of the pesticides studied had recoveries between 81 and 110%, 98% of the pesticides had intermediate precision of <or=20%, and 95% of the pesticides showed measurement uncertainty of <or=40%. Compared to LC/ESI-MS/MS, UHPLC QqTOF MS showed a relatively poor repeatability and large measurement uncertainty. Ninety-five percent of the pesticides analyzed by UHPLC QqTOF MS had recoveries between 81 and 110%, 86% of the pesticides had intermediate precision of <or=20%, and 83% of the pesticides showed measurement uncertainty of <or=40%. LC/ESI-MS/MS proved to be the first choice for quantification or pretarget analysis due to its superior sensitivity and good repeatability. UHPLC QqTOF MS provided accurate mass measurement and was an ideal tool for post-target screening and confirmation.
本研究介绍了液相色谱-电喷雾串联质谱（LC/ESI-MS/MS）和超高效液相色谱-电喷雾四极杆飞行时间质谱（UHPLC QqTOF MS）在测定浆果中 148 种农药中的应用。采用 QuEChERS（快速、简单、廉价、有效、耐用和安全）法从浆果中提取农药。采用基质匹配标准校准曲线，使用同位素标记标准品或化学类似物作为内标进行定量，分析范围为 5 至 500μg/kg。方法性能参数，包括总回收率、中间精密度和测量不确定度，根据设计实验，即嵌套设计进行评估。对于 LC/ESI-MS/MS，研究的 95%的农药回收率在 81%至 110%之间，98%的农药中间精密度<或=20%，95%的农药测量不确定度<或=40%。与 LC/ESI-MS/MS 相比，UHPLC QqTOF MS 显示出相对较差的重复性和较大的测量不确定度。95%的通过 UHPLC QqTOF MS 分析的农药回收率在 81%至 110%之间，86%的农药中间精密度<或=20%，83%的农药测量不确定度<或=40%。由于其灵敏度高、重复性好，LC/ESI-MS/MS 被证明是定量或预靶向分析的首选方法。UHPLC QqTOF MS 提供了准确的质量测量，是用于后靶向筛选和确证的理想工具。
