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目的建立食品包装材料中三甲基锡(TMT)、三丁基锡(TBT)和三苯基锡(TPh T)迁移量的超高效液相色谱-串联质谱联用法(UPLC-MS/MS)。方法在水、10%(v/v)乙醇溶液和3%(w/v)乙酸溶液3种食品模拟物中加入0.125 mol/L盐酸溶液,使有机锡化合物呈阳离子态,经阳离子固相萃取柱净化富集,洗脱液在40℃水浴下氮气吹干;正己烷食品模拟物直接在40℃水浴下氮气吹干。残渣用流动相溶解,旋涡混匀60 s,过0.22μm微孔滤膜,经C18色谱柱分离,串联质谱仪上采用多反应监测正离子模式测定,外标法定量。结果 3种有机锡化合物在1.0~100μg/L范围内相关系数大于0.999 8,检出限为0.1~0.3μg/L。平均回收率,三甲基锡为90.6%~97.3%、三丁基锡为89.5%~94.1%,三苯基锡为88.6%~96.0%。RSD小于6.7%。结论本法快速简便、准确,可用于测定食品包装材料三甲基锡、三丁基锡和三苯基锡的迁移量。
Objective To establish a UPLC-MS / MS method for the migration of TMT, TBT and TPh T in food packaging materials. Methods 0.125 mol / L hydrochloric acid solution was added to three kinds of food simulants including water, 10% (v / v) ethanol solution and 3% (w / v) acetic acid solution to make the organotin compounds in cationic state. Column purification enrichment, the eluent was dried under nitrogen at 40 ℃ water bath; n-hexane food simulants were directly dried under nitrogen at 40 ℃ water bath. The residue was dissolved in the mobile phase, vortexed for 60 s, filtered through a 0.22 μm microporous membrane and separated on a C18 column. Multiple tandem mass spectrometry was used to determine the positive ion mode and the external standard method was used. Results The correlation coefficient of three organotin compounds in the range of 1.0-100 μg / L was greater than 0.999 8 and the detection limit was 0.1-0.3 μg / L. The average recovery was 90.6% -97.3% for trimethyltin, 89.5% -94.1% for tributyltin, and 88.6% -96.0% for triphenyltin. RSD less than 6.7%. Conclusion This method is rapid, simple and accurate and can be used to determine the migration of trimethyltin, tributyltin and triphenyltin in food packaging materials.