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基于 ZrO2 的固相萃取/QuEChERS 用高效液相色谱-二极管阵列检测法在 d-SPE 净化步骤中用于食用油中农药分析。

Application of HPLC-DAD after SPE/QuEChERS with ZrO2-based sorbent in d-SPE clean-up step for pesticide analysis in edible oils.

机构信息

Medical University in Lublin, Faculty of Pharmacy with Medical Analytics Division, Chair of Chemistry, Department of Physical Chemistry, 4A Chodźki Street, 20-093 Lublin, Poland.

Medical University in Lublin, Faculty of Pharmacy with Medical Analytics Division, Chair of Chemistry, Department of Physical Chemistry, 4A Chodźki Street, 20-093 Lublin, Poland.

出版信息

Food Chem. 2016 Jan 1;190:71-79. doi: 10.1016/j.foodchem.2015.05.072. Epub 2015 May 18.

DOI:10.1016/j.foodchem.2015.05.072
PMID:26212943
Abstract

In this study, the solid-phase extraction/quick, easy, cheap, effective, rugged and safe (SPE/QuEChERS) technique was adapted to develop a simple sample treatment for multi-residue pesticide analysis of edible oils. The proposed method is based on liquid-liquid partitioning with acetonitrile followed by dispersive solid phase extraction using zirconia-coated silica particles for extract purification. To evaluate the described method, 21 pesticides belonging to different chemical classes were analysed using high performance liquid chromatography with diode-array detection (HPLC-DAD). For validation purposes, recovery studies were performed at 75 ng g(-1), 125 ng g(-1), 250 ng g(-1), 500 ng g(-1) and 1000 ng g(-1) levels. Recoveries were over the range of 50-130% for most of the analytes, with relative standard deviations less than 15% being observed. HPLC-DAD provided suitable linearity, precision and accuracy. The validated method was successfully applied to the analysis of edible oil samples selected from the market.

摘要

本研究采用固相萃取/快速、简便、廉价、有效、耐用、安全(SPE/QuEChERS)技术,开发了一种用于食用油中多残留农药分析的简单样品处理方法。该方法基于乙腈的液-液分配,然后使用氧化锆涂覆的硅胶颗粒进行分散固相萃取,以净化提取物。为了评估所描述的方法,使用高效液相色谱-二极管阵列检测(HPLC-DAD)分析了属于不同化学类别的 21 种农药。为了验证目的,在 75ng g(-1)、125ng g(-1)、250ng g(-1)、500ng g(-1)和 1000ng g(-1)水平进行了回收率研究。大多数分析物的回收率在 50-130%之间,相对标准偏差小于 15%。HPLC-DAD 提供了合适的线性度、精密度和准确度。该经验证的方法成功应用于市场上选择的食用油样品的分析。

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