【摘要】 建立了葡萄酒中三甲基锡、二甲基锡和一甲基锡同时检测的四乙基硼化钠衍生/顶空气相色谱-火焰光度检测法。对顶空条件(温度、时间、振荡方式)、衍生化条件(试剂用量、p H值、盐度)以及气相色谱条件进行了优化。在最佳实验条件下,葡萄酒中3种甲基锡化合物的检出限(LOD)分别为1.2,1.0,1.2μg/kg;干白、干红和桃红3种代表性葡萄酒样品在5.0,10.0,100.0μg/kg加标水平下的平均回收率为80.5%~101.4%,相对标准偏差(RSD,n=6)为3.2%~8.5%。该方法具有良好的灵敏度和准确度,操作简单、快速,单个样品的平均分析时间不超过25 min,适用于葡萄酒中甲基锡化合物的快速筛查检测。更多还原

【Abstract】 A method for the simultaneous determination of trimethyltin( TMT),dimethyltin( DMT)and monomethyltin( MMT) in wine was developed by headspace extraction coupled with gas chromatography and flame photometric detection( GC- FPD) after in-situ derivatization with sodium tetraethylborate( Na BEt4). The headspace conditions( temperature,time and oscillating mode),derivatization parameters( amount of Na BEt4,p H value and salinity) and GC conditions were optimized. In the optimal experimental conditions,the limits of detection( LODs) were 1. 2,1. 0,1. 2 μg / kg for TMT,DMT and MMT,respectively. For the three representative matrices of dry white,dry red and pink wine,the average recoveries at three spiked levels of 5. 0,10. 0,100. 0 μg / kg were in the range of 80. 5%- 101. 4%,and the relative standard deviations( RSDs,n = 6) ranged from 3. 2% to8. 5%. The proposed method was validated to have high sensitivity and high accuracy,also with the special advantages of simplicity and rapidness. The total analysis time for one sample is not more than 25 min by the proposed method,and it is suitable for the rapid screening of methyltin compounds in wine.更多还原