高效液相色谱-串联质谱法测定植物性食品中多种有机锡化合物  

Determination a Variety of Organotin Compounds in Foodstuffs of Plant Origin by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：石声鑫 杨建英 徐宁 陈晓红 陈庆 肖晓槟 SHI Shengxin;YANG Jianying;XU Ning;CHEN Xiaohong;CHEN Qing;XIAO Xiaobin(Guangdong Shantou Supervision Testing Institute of Quality and Metrology,Shantou 515041,China)

机构地区：[1]广东省汕头市质量计量监督检测所,广东汕头515041

出　　处：《现代食品》2024年第1期195-200,共6页Modern Food

基　　金：广东省市场监督管理局2023年度科技项目(2023CS09)。

摘　　要：样品分别经甲酸乙腈(甲酸1%)和甲酸甲醇(甲酸1%)提取,上清提取液经混合盐析试剂除水分层,上清液与水按2∶3(体积比)混合,过膜后上机检测。以0.2 g·L^(-1)乙酸铵水溶液(含0.1%甲酸)-0.1%甲酸乙腈为流动相,在0.3 mL·min^(-1)流速下梯度洗脱,采用苯基色谱柱进行液相分离,正离子模式检测,外标法定量。结果表明,在草莓、苹果、柑橘、葡萄、黄瓜5种基质中,7种有机锡化合物线性关系良好,相关系数均≥0.995;方法检出限为0.2~4μg·kg^(-1),定量下限为0.5~10μg·kg^(-1);在3个浓度添加水平下,7种有机锡化合物的平均回收率为68.1%~103.1%,相对标准偏差为1.00%~11.36%。该方法准确、灵敏、快捷,适用于植物源性食品中多种有机锡化合物的定量分析。The samples were extracted with formic acid acetonitrile(1%formic acid)and formic acid methanol(1%formic acid),respectively.The supernatant extract was dehydrated and layered using a mixed salt precipitation reagent.The supernatant was mixed with water in a ratio of 2∶3(volume ratio),and then subjected to membrane filtration and machine detection.Using 0.2 g·L^(-1) ammonium acetate aqueous solution(containing 0.1%formic acid)-0.1%formic acid acetonitrile as the mobile phase,gradient elution was performed at a flow rate of 0.3 mL·min^(-1).A benzene chromatography column was used for liquid phase separation,positive ion mode detection,and external standard quantification.The results showed that among the five substrates of strawberries,apples,citrus,grapes,and cucumbers,seven organic tin compounds had a good linear relationship,with correlation coefficients≥0.995;the detection limit of the method is 0.2~4μg·kg^(-1),lower limit of quantification is 0.5~10μg·kg^(-1);at three levels of concentration addition,the average recovery rates of seven organotin compounds were 68.1%~103.1%,with a relative standard deviation of 1.00%to 11.36%.This method is accurate,sensitive,and fast,and is suitable for quantitative analysis of various organic tin compounds in plant-based foods.

关 键 词：高效液相色谱-串联质谱法 有机锡化合物 植物性食品 

分 类 号：O657.7[理学—分析化学]