Instituto de Química, Universidade Estadual de Campinas, Campinas, SP, Brazil.
J Sep Sci. 2018 Apr;41(8):1726-1733. doi: 10.1002/jssc.201701038. Epub 2018 Feb 7.
A new analytical method for multiresidue determination of 16 multiclass pesticides in lettuce was developed using ultra-high performance liquid chromatography with tandem mass spectrometry with a triple quadrupole mass analyzer and positive mode electrospray ionization, using a previously optimized quick, easy, cheap, effective, rugged, and safe method for sample preparation. Validation studies, according to document SANTE/11945/2015, demonstrated that the developed method is selective, accurate, and precise, providing recoveries of 70-120%, relative standard deviations ≤20% and quantification limits from 3 μg/kg. The method was compared with one based on high-performance liquid chromatography with tandem mass spectrometry, in terms of chromatographic performance, detectability and matrix effect for five varieties of lettuce. The new method provided a reduction in the time for the chromatographic analysis of 50%, from 30 to 15 min, using a lower mobile phase flow rate (0.147 mL/min), which reduced the consumption of mobile phase by 25%, and injection of smaller amounts of sample (1.7 μL). Lower limits of quantification were obtained for almost all pesticides studied for green-leaf lettuce. However, in relation to the matrix effect, four of the five types of lettuce studied presented higher matrix effects.
采用三重四极杆质谱仪和正离子电喷雾电离源的超高效液相色谱-串联质谱法，结合之前优化的快速、简便、廉价、有效、耐用和安全的样品前处理方法，建立了一种同时测定生菜中 16 种多类农药残留的多残留分析方法。按照 SANTE/11945/2015 号文件进行验证研究表明，该方法具有选择性、准确性和精密度，回收率为 70-120%，相对标准偏差≤20%，定量限为 3μg/kg。在色谱性能、检测能力和五种生菜基质效应方面，将该方法与基于高效液相色谱-串联质谱法的方法进行了比较。新方法通过使用较低的流动相流速（0.147mL/min），将色谱分析时间从 30 分钟缩短至 15 分钟，减少了 25%的流动相消耗，并减少了 1.7μL 的样品进样量，从而将 50%的色谱分析时间缩短。对于几乎所有研究的绿叶生菜农药，都获得了更低的定量限。然而，就基质效应而言，所研究的五种生菜中有四种呈现出更高的基质效应。
