Canadian Food Inspection Agency Calgary Laboratory, Calgary, Alberta, Canada.
J Agric Food Chem. 2011 Aug 24;59(16):8589-608. doi: 10.1021/jf202158g. Epub 2011 Aug 3.
A comparison of ultrahigh performance liquid chromatography (UHPLC) with a 2.6 μm core-shell particle column (Kinetex C(18)) and conventional liquid chromatography (LC) with a 3 μm porous particle column (Atlantis dC(18)), coupled with electrospray ionization tandem mass spectrometry (ESI-MS/MS), for the determination of 151 pesticides in grains is presented in this study. Pesticides were extracted from grain samples using a procedure known as QuEChERS (quick, easy, cheap, effective, rugged, and safe). Quantification, with an analytical range from 5 to 500 μg/kg, was achieved using matrix-matched standard calibration curves with isotopically labeled standards or a chemical analogue as internal standards. The method performance parameters that included overall recovery, intermediate precision, and measurement uncertainty were evaluated using a designed experiment, that is, the nested design. The UHPLC (Kinetex C(18)) was superior to conventional LC (Atlantis dC(18)) as it yielded a shorter analytical run time, increased method sensitivity, and improved method performance. For UHPLC/ESI-MS/MS (Kinetex C(18)), 90% of the pesticides studied had recoveries between 81 and 110%, 88% of the pesticides had intermediate precision ≤20%, and 84% of the pesticides showed measurement uncertainty ≤40%. As compared to UHPLC/ESI-MS/MS (Kinetex dC(18)), the LC/ESI-MS/MS (Atlantis dC(18)) showed a relatively lower sensitivity, less repeatability, and larger measurement uncertainty. UHPLC/ESI-MS/MS with 2.6 μm core-shell particle column and scheduled MRM proved to be a good choice for quantification or determination of pesticides in grains.
本研究比较了超高效液相色谱（UHPLC）与 2.6μm 核壳颗粒柱（Kinetex C(18)）和常规液相色谱（LC）与 3μm 多孔颗粒柱（Atlantis dC(18)），结合电喷雾串联质谱（ESI-MS/MS），用于谷物中 151 种农药的测定。采用 QuEChERS（快速、简单、廉价、有效、坚固、安全）法从谷物样品中提取农药。采用基质匹配标准校准曲线和同位素标记标准或化学类似物作为内标进行定量，分析范围为 5 至 500μg/kg。使用嵌套设计的设计实验评估了方法性能参数，包括总回收率、中间精密度和测量不确定度。与常规 LC（Atlantis dC(18)）相比，UHPLC（Kinetex C(18)）具有较短的分析运行时间、更高的方法灵敏度和更好的方法性能。对于 UHPLC/ESI-MS/MS（Kinetex C(18)），90%的研究农药的回收率在 81%至 110%之间，88%的农药的中间精密度≤20%，84%的农药的测量不确定度≤40%。与 UHPLC/ESI-MS/MS（Kinetex dC(18)）相比，LC/ESI-MS/MS（Atlantis dC(18)）的灵敏度相对较低、重复性较差、测量不确定度较大。采用 2.6μm 核壳颗粒柱和预定 MRM 的 UHPLC/ESI-MS/MS 被证明是谷物中农药定量或测定的良好选择。
