Li Hui, Jiang Zejun, Cao Xiaolin, Su Hang, Shao Hua, Jin Fen, Abd El-Aty A M, Wang Jing
Institute of Quality Standard and Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences, Key Laboratory of Agro-product Quality and Safety, Ministry of Agriculture, Beijing, 100081, PR China.
Department of Pharmacology, Faculty of Veterinary Medicine, Cairo University, 12211, Giza, Egypt; Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul, 143-701, Republic of Korea.
J Chromatogr A. 2017 Dec 15;1528:53-60. doi: 10.1016/j.chroma.2017.10.075. Epub 2017 Nov 2.
Herein, an accurate and reliable isotope-labelled internal standard method was developed and validated for simultaneous determination of three polar pesticide adjuvants, namely 2-pyrrolidone, N-methyl-2-pyrrolidone, and N-ethyl-2-pyrrolidone in plant-derived agro-products. Matrices, including apple, cabbage, tomato, cucumber, rice, and wheat were extracted with a modified quick, easy, cheap, effective, rugged, and safe "QuEChERS" method and purified with a new clean-up sorbent (Z-Sep). A hydrophilic interaction liquid chromatography column (HILIC), exhibiting a lipophilic-hydrophilic character, was used to separate the three analytes over 10min using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Matrix effects in various matrices were evaluated and an isotope-labelled internal standard method was employed to compensate for ion enhancement/suppression effects. At three fortification levels (2.0, 5.0, and 20.0μg/kg), the mean recoveries ranged from 78.5 to 112.1% with relative standard deviations (RSDs)<11.0% for all tested analytes. The limits of detection (LODs) and quantification (LOQs) were 0.04-0.45 and 0.12-1.58μg/kg in various matrices, respectively. The developed experimental protocol was successfully applied to monitor different samples purchased from local markets in Beijing, China. In conclusion, the developed method exhibited both high sensitivity and satisfactory accuracy and is suitable for the simultaneous determination of the three tested pesticide adjuvant residues in agro-products of plant origin.
本文建立并验证了一种准确可靠的同位素标记内标法，用于同时测定植物源农产品中的三种极性农药助剂，即2-吡咯烷酮、N-甲基-2-吡咯烷酮和N-乙基-2-吡咯烷酮。采用改良的快速、简便、廉价、高效、耐用且安全的“QuEChERS”方法对苹果、卷心菜、番茄、黄瓜、大米和小麦等基质进行提取，并用新型净化吸附剂（Z-Sep）进行净化。使用具有亲脂-亲水特性的亲水作用液相色谱柱（HILIC），通过液相色谱-串联质谱（LC-MS/MS）在10分钟内分离这三种分析物。评估了各种基质中的基质效应，并采用同位素标记内标法来补偿离子增强/抑制效应。在三个加标水平（2.0、5.0和20.0μg/kg）下，所有测试分析物的平均回收率在78.5%至112.1%之间，相对标准偏差（RSDs）<11.0%。在各种基质中，检测限（LODs）和定量限（LOQs）分别为0.04 - 0.45和0.12 - 1.58μg/kg。所建立的实验方案成功应用于监测从中国北京当地市场购买的不同样品。总之，所建立的方法具有高灵敏度和令人满意的准确度，适用于同时测定植物源农产品中三种测试农药助剂残留。
