Wang Jian, Leung Daniel
Canadian Food Inspection Agency, Calgary Laboratory, Calgary, Alberta, Canada.
J Agric Food Chem. 2009 Mar 25;57(6):2162-73. doi: 10.1021/jf803419j.
The applications of ultra-performance liquid chromatography electrospray ionization quadrupole time-of-flight mass spectrometry (UPLC QqTOF) in the determination of 138 pesticides in fruit- and vegetable-based infant foods were investigated. Pesticides were extracted from infant foods using a procedure known as the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. UPLC QqTOF MS full-scan with a relatively high sensitivity proved to be an ideal tool for screening of a large number of pesticides in a single analysis. UPLC QqTOF MS/MS provided product ion spectra that allowed for unequivocal confirmation of pesticides. Quantification 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 according to a designed experiment, that is, the nested design. Generally, about 90% of the pesticides studied had recoveries between 81 and 110%, 90% had intermediate precision of <or=25%, and 85% had measurement uncertainty of <or=50%. Compared to LC-ESI-MS/MS, UPLC QqTOF MS showed a relatively poor repeatability and large measurement uncertainty for quantification. In general, UPLC QqTOF can be used for screening, quantifying, and confirming pesticides in infant foods at 10 microg/kg.
研究了超高效液相色谱-电喷雾电离-四极杆飞行时间质谱法(UPLC QqTOF)在测定果蔬类婴儿食品中138种农药的应用。采用一种名为快速、简便、廉价、高效、耐用和安全(QuEChERS)的方法从婴儿食品中提取农药。结果表明,具有较高灵敏度的UPLC QqTOF MS全扫描是在单次分析中筛选大量农药的理想工具。UPLC QqTOF MS/MS提供的产物离子谱可明确确认农药。使用与基质匹配的标准校准曲线,并以同位素标记标准品或化学类似物作为内标进行定量。根据设计的实验即嵌套设计,评估了包括总回收率、中间精密度和测量不确定度在内的方法性能参数。一般来说,所研究的农药中约90%的回收率在81%至110%之间,90%的中间精密度≤25%,85%的测量不确定度≤50%。与LC-ESI-MS/MS相比,UPLC QqTOF MS在定量方面的重复性相对较差,测量不确定度较大。总体而言,UPLC QqTOF可用于筛查、定量和确认婴儿食品中含量为10微克/千克的农药。