气质联用法测定甜瓜中代森锌  

Determination of Dithane Z-78 Residues in Muskmelon by Gas Chromatography-tandem Mass Spectrometry

作　　者：帕尔哈提·克依木[1] 周晓龙[1] 刘河疆[1] 

机构地区：[1]新疆农业科学院农业质量标准与检测技术研究所,农业部农产品质量安全风险评估实验室(乌鲁木齐),新疆农产品质量安全实验室,新疆乌鲁木齐830091

出　　处：《食品研究与开发》2017年第17期134-138,共5页Food Research and Development

基　　金：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);新疆维吾尔自治区公益性科研院所基本科研业务经费资助项目(KYGY2016110);新疆维吾尔自治区高技术研究发展计划项目(201517106)

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。A rapid determination method of Dithane Z-78 residues in muskmelon was established by gas chromatography-tandem mass spectrometry（GC-MS/MS）. Orthogonal experimental design,was used to reaction with the SnCl_2-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 determination.The results showed that the optimized conditions of pretreatment was using hexane as extraction solvent,ultrasonic time was 45 min,water temperature was 60 ℃,sample weight was 10 g,and ascorbic acid content 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 average 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.

关 键 词：代森锌 正交试验 气质联用 甜瓜 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]