中文摘要：本文构建了一个水果和果浆中农药（马拉硫磷、二嗪磷、吡虫啉、三唑酮）残留全自动检测方法，该程序以乙腈为水混有机溶剂进行液-液萃取，然后以葡萄糖为糖析出剂进行相分离，最后将含有农药的提取液注入高效液相色谱-串联质谱系统进行检测。该自动化样本制备过程快速、简单、低廉且可避免传统液-液萃取的缺点。在优化的实验条件下，马拉硫磷和三唑酮的线性检测范围为0.01-10mg/L, 二嗪磷的线性检测范围为0.001-10mg/L, 吡虫啉的线性检测范围为0.1-10mg/L，检测限分别为0.003、0.0003和0.03mg/L。该方法已经成功地应用于五种市售水果和果浆样本中四种农药残留检测，分析结果与气相色谱法火焰离子化检测器检测结果相吻合。
外文摘要：A fully automated method for the determination of pesticides (malathion, diazinon, imidacloprid and triadimefon) in fruit and berry juices has been developed. In the current study, the on-line in-syringe sugaring-out liquid-liquid extraction was successfully combined with a HPLC-MS/MS system for the first time. The procedure assumes the liquid-liquid extraction of analytes in water-miscible organic solvent acetonitrile followed by phase separation using glucose as sugaring-out reagent. After the phase separation in a syringe of a flow system, the extract containing pesticides was injected into the HPLC-MS/MS system.The proposed automated sample preparation procedure is rapid, simple, relatively inexpensive, and allows to avoid shortcomings of conventional liquid-liquid extraction, such as necessity to use nonpolar organic solvents, which are not always suitable for the HPLC-MS/MS detection. The conditions of pesticides' extraction such as ratio of acetonitrile/water, type and concentration of sugaring-out reagent, volume of sample and effect of pH have been studied and optimized. Under optimal experimental conditions the linear detection ranges were found to be 10(-2)-10 mg L-1 for malathion and triadimefon, 10(-3)-10 mg L-1 for diazinon, and 10(-1)-10 mg L-1 for imidacloprid. The LODs, calculated from a blank test, based on 3 sigma, found to be 3.10(-3) mg L-1 for malathion and triadimefon, 3.10(-4) mg L-1 for diazinon and 3.10(-2) mg L-1 for imidacloprid. The application of the method has been demonstrated in the determination of these four pesticides in commercial samples of five fruit and berry juices. As an outcome, the analyticalresults agreed fairly well with the results obtained by a reference GCFID method.
 
外文关键词：Pesticides, Juices, In-syringe sugaring-out liquid-liquid extraction, Flow system, HPLC-MS/MS
作者：Timofeeva, Irina; Shishov, Andrey; Kanashina, Dania; Dzema, Dania; Bulatov, Andrey
作者单位：St Petersburg State Univ SPbSU, St Petersburg Univ SPbU, Inst Chem, Dept Analyt Chem, 7-9 Univ Skaya Nab, St Petersburg 199034, Russia.
期刊名称：TALANTA
期刊影响因子：4.035
出版年份：2017
出版刊次：3
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