A Modified QuEChERS Extraction and LC-MS/MS Method for the Determination of Pesticide Residues in Curry Leaves (Murraya koenigii)

Ranjith Arimboor, K. R. Menon, N. Babu, Haneesh Chandran
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引用次数: 2

Abstract

Increased consumer demand for curry leaves free from pesticides demands fast and reliable analytical methods for the analysis of pesticide residues.The optimization of a QuEChERS based sample preparation technique with improved analytical accuracy by removing interfering matrix components for LC-MS/MS analysis of pesticide residues from curry leaves.A modified QuEChERS solid phase extraction method was developed and validated for the analysis of 26 pesticides in fresh and dried curry leaves. The effects of the sample preparation steps and column retention time on the matrix suppression of analyte ions were also evaluated.Validation parameters were found within an acceptable range. The matrix effect evaluation studies showed that the QuEChERS sample preparation was able to minimize the ion suppression of analytes due to co-eluting matrix of components and that a d-SPE clean up step had major role in reducing matrix effect. The gradient mobile phase with longer retention time for analytes resulted in comparatively lesser matrix effects than the isocratic mobile phase of non-polar nature. Even after the clean up, a considerable number of compounds had more than 20% reduction in their MS response in the gradient mobile phase.This study emphasized the need of proper sample clean up before a LC-MS/MS analysis and the usage of matrix matched standards and mobile phase that ultimately results in an appropriate analyte separation in reasonable retention times.
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改良QuEChERS萃取- LC-MS/MS法测定咖喱叶中农药残留
消费者对无农药咖喱叶的需求不断增加,对快速、可靠的农药残留分析方法提出了要求。基于QuEChERS的样品制备技术优化,去除干扰基质成分,提高分析精度,用于hplc -MS/MS分析咖喱叶中农药残留。建立了一种改进的QuEChERS固相萃取法,并对鲜咖喱叶和干咖喱叶中26种农药进行了分析。考察了样品制备步骤和柱保留时间对基质抑制分析离子的影响。验证参数在可接受范围内。基质效应评价研究表明,QuEChERS样品制备能够最大限度地减少组分基质共洗脱对分析物的离子抑制,d-SPE清理步骤对降低基质效应起主要作用。与非极性等压流动相相比,具有较长停留时间的梯度流动相的基质效应相对较小。即使在清理后,相当多的化合物在梯度流动相的MS响应也降低了20%以上。本研究强调在LC-MS/MS分析前需要适当的样品清理,使用基质匹配的标准品和流动相,最终在合理的保留时间内得到适当的分析物分离。
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