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采用 QuEChERS-UHPLC-MS/MS 法测定生菜中多种农药残留量的分析方法的建立与验证。

Development and validation of an analytical method for multiresidue determination of pesticides in lettuce using QuEChERS-UHPLC-MS/MS.

机构信息

Instituto de Química, Universidade Estadual de Campinas, Campinas, SP, Brazil.

出版信息

J Sep Sci. 2018 Apr;41(8):1726-1733. doi: 10.1002/jssc.201701038. Epub 2018 Feb 7.

Abstract

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.

摘要

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。

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