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建立一种 GC-MS 方法用于检测蔬菜水果中代森锰锌等二硫代氨基甲酸酯类杀菌剂残留量及其安全性评估。

Validation of a GC-MS method for the estimation of dithiocarbamate fungicide residues and safety evaluation of mancozeb in fruits and vegetables.

机构信息

National Referral Laboratory, National Research Centre for Grapes, P.O. Manjri Farm, Pune 412 307, India.

Centro de Investigación en Contaminación Ambiental (CICA), Universidad de Costa Rica, P.O. 2060 San José, Costa Rica.

出版信息

Food Chem. 2014 May 1;150:175-81. doi: 10.1016/j.foodchem.2013.10.148. Epub 2013 Nov 1.

Abstract

A sensitive and rugged residue analysis method was validated for the estimation of dithiocarbamate fungicides in a variety of fruit and vegetable matrices. The sample preparation method involved reaction of dithiocarbamates with Tin(II) chloride in aqueous HCl. The CS2 produced was absorbed into an isooctane layer and estimated by GC-MS selected ion monitoring. Limit of quantification (LOQ) was ⩽40μgkg(-1) for grape, green chilli, tomato, potato, brinjal, pineapple and chayote and the recoveries were within 75-104% (RSD<15% at LOQ). The method could be satisfactorily applied for analysis of real world samples. Dissipation of mancozeb, the most-used dithiocarbamate fungicide, in field followed first+first order kinetics with pre-harvest intervals of 2 and 4days in brinjal, 7 and 10days in grapes and 0day in chilli at single and double dose of agricultural applications. Cooking practices were effective for removal of mancozeb residues from vegetables.

摘要

建立了一种用于多种水果蔬菜基质中二硫代氨基甲酸盐类杀菌剂残留分析的高灵敏度、强耐用性的检测方法。样品前处理方法是二硫代氨基甲酸盐与氯化亚锡在盐酸水溶液中发生反应,生成的二硫化碳(CS2)用异辛烷萃取后,采用气相色谱-质谱选择离子监测(GC-MS-SIM)模式进行定量分析。葡萄、青椒、番茄、土豆、茄子、菠萝和佛手瓜中,二硫代氨基甲酸盐类杀菌剂的定量限(LOQ)均小于 40μgkg(-1),在 LOQ 处的回收率为 75%-104%(RSD<15%)。该方法可用于实际样品的分析。在田间条件下,二硫代氨基甲酸盐类杀菌剂代森锰锌在茄子中的消解符合一级+一级动力学模型,在葡萄中的消解符合一级动力学模型,其半衰期分别为 2d 和 4d、7d 和 10d,在辣椒中的消解符合零级动力学模型。在农业实际使用剂量下,半衰期分别为 1d 和 2d。烹饪处理可以有效去除蔬菜中的代森锰锌残留。

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