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投稿时间：2017-06-05
投稿时间：2017-06-05
中文摘要: 建立一种气质联用法快速测定甜瓜中代森锌残留量的方法。通过进行正交试验优化，采用超声反应提取方 式，在密闭反应瓶内用氯化亚锡盐酸溶液对甜瓜中残留的代森锌进行还原反应，将生成的二硫化碳用正己烷吸收，用 气相色谱串联质谱 SIM 模式采集数据，外标法定量，间接测定甜瓜中代森锌残留量。样品前处理优化条件为正己烷 做吸收溶剂，水浴超声时间为 45 min，超声温度为 60 ℃，称样量为 10 g，抗坏血酸添加量为 0.1 g。该方法在 0.3 mg/kg～ 20 mg/kg 范围内具有良好的线性关系，相关系数大于 0.991，在添加量范围平均回收率为 71.0 %～90.8 %，变异系数（RSD）为 0.5 %，最小检出限在 0.2 mg/kg，最小定量限为 0.67 mg/kg。
Abstract:A rapid determination method of Dithane Z-78 residues in muskmelon was established by gas chro－ matography-tandem mass spectrometry （GC-MS/MS）. Orthogonal experimental design，was used to reaction with the SnCl2-HCl solution in the sample bottle by ultrasonic extraction. Then CS2， was extracted by hexane， which，was detected by using SIM mode of the GC-MS/MS， external standards were used for quantitative deter－ mination.The results showed that the optimized conditions of pretreatment was using hexane as extraction sol－ vent， ultrasonic time was 45 min，water temperature was 60 ℃， sample weight was 10 g，and ascorbic acid con－ tent was 0.1g. This method was showed good linearity in the range of 0. 3 mg/kg to 20 mg/kg（r=0.991），the aver－ age recoveries of all the spiked levels were in the range of 71.0 % to 90.8 %， the RSD were 0.5 %； The limit of detection（LOD）was below 0. 2 mg/kg and the limit of quantity was below 0. 67 mg/kg.
keywords: Dithane Z-78 orthogonal experimental design gas chromatography-tandem mass spectrometry muskmelon
文章编号：201717030 中图分类号： 文献标志码：A
基金项目:新疆维吾尔自治区公益性科研院所基本科研业务经费资助项目（KY2017055）；新疆维吾尔自治区高技术研究发展计划项目
（201517106）；新疆维吾尔自治区公益性科研院所基本科研业务经 费资助项目（KYGY2016110）
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