Srivastava Neha, Kumari Supriya, Nair Kishore, Alam Samsul, Raza Syed K
Institute of Pesticide Formulation Technology, Analytical Division, Sector-20, Udyog Vihar, Opposite Ambience Mall, NH-8 Gurgaon, Haryana, India.
J AOAC Int. 2017 May 1;100(3):804-809. doi: 10.5740/jaoacint.16-0312. Epub 2017 Jan 12.
The present paper depicts a novel method based on magnetic SPE (MSPE) for the determination of organophosphorus pesticides (OPs) such as phorate, malathion, and chlorpyrifos in environmental water samples. In this study, C18 functionalized silica-coated core-shell iron oxide magnetic nanoparticles (MNPs) were used as a surface-engineered magnetic sorbent for the selective extraction of pesticides from aqueous samples, followed by GC-MS and GC-tandem MS analysis for confirmative determination of the analytes. Various important method parameters, including quantity of MNP adsorbent, volume of sample, effective time for extraction, nature of the desorbing solvent, and pH of the aqueous sample, were investigated and optimized to obtain maximum method performance. Under the optimized instrumental analysis conditions, good linearity (r2 value ≥0.994) was achieved at the concentration range of 0.5-500 μg/L. Recoveries were in the range of 79.2-96.3 and 80.4-97.5% in selective-ion monitoring and multiple reaction monitoring (MRM) modes, respectively, at the spiking concentrations of 1, 5, and 10 μg/L. MRM mode showed better sensitivity, selectivity, and low-level detection (0.5 μg/L) of analytes. The novel MSPE method is a simple, cheap, rapid, and eco-friendly method for the determination of OPs in environmental water samples.
本文描述了一种基于磁性固相萃取(MSPE)的新方法,用于测定环境水样中的有机磷农药(OPs),如甲拌磷、马拉硫磷和毒死蜱。在本研究中,C18功能化的二氧化硅包覆的核壳型氧化铁磁性纳米颗粒(MNPs)被用作表面工程化磁性吸附剂,用于从水样中选择性萃取农药,随后进行气相色谱-质谱联用(GC-MS)和气相色谱-串联质谱(GC-MS/MS)分析,以确证测定分析物。研究并优化了各种重要的方法参数,包括MNP吸附剂的用量、样品体积、有效萃取时间、解吸溶剂的性质以及水样的pH值,以获得最佳的方法性能。在优化的仪器分析条件下,在0.5-500μg/L的浓度范围内实现了良好的线性(r2值≥ 0.994)。在1、5和10μg/L的加标浓度下,选择性离子监测和多反应监测(MRM)模式下的回收率分别在79.2-96.3%和80.4-97.5%的范围内。MRM模式对分析物显示出更好的灵敏度、选择性和低水平检测能力(0.5μg/L)。这种新的MSPE方法是一种用于测定环境水样中OPs的简单、廉价、快速且环保的方法。