【摘要】 [目的]采用四乙基硼化钠(STEB)衍生化,建立一个简单、高效的水产品中有机锡残留气相色谱-质谱联用仪(GC-MS)测定方法,以满足实验室日常检测的需要。[方法]采用酸性甲醇[含环庚酸烯酚酮(Tropolone)]超声波提取,C-18固相萃取净化,STEB衍生化,GC-MS检测,内标法定量。[结果]通过有效的净化和衍生化的优化,使STEB衍生化方法所具有的快速简单等优越性在复杂基质(有机锡类化合物,OT)样品检测中得到体现,该方法的最低检测限为2ng/g(OT的定量以Sn计),测定标准参考物ERM-CE477,测量值与鉴定值的偏差小于5%,5个平行样测量值的标准偏差除二苯基锡(DPT)(14.8%)外都在8%以内。[结论]本方法是一项测定水产品中OT残留量的快速、有效、可靠的方法,为水产品中OT残留量监测提供了技术保证。更多还原

【Abstract】 [Objective] To develop a method for simple and rapid determination of organo-tin residues in aquatic products by gas chromatography-mass spectrometer(GC-MS)coupling with Sodium tetraethylborate derivatization.[Methods] Hydrolyzation and extraction of sample was performed with acetic acid methanol containing 0.005% tropolone firstly,then clean-up was done with C-18 solid phase extraction(SPE),after that,derivatizative reaction was performed with sodium tetraethylborate,and then sample was qualified and quantified(internal standard method)with GC-MS finally.[Results] Due to action of tropolone to organo-tin in clean-up,less methanol was used in eluted solution,by which more matrix that inhibited derivatization was kept in column and recovery of organo-tin was very good.Limit of detection(LOD)was 2 ng/g,5 parallel samples of reference standard ERM-CE477 were determined,the result showed very well with 2.8%-14.8% of relative standard deviation(RSD)range and less than 5% difference to certified value.[Conclusion] The method provided technical base for organo-tin standard analytical method.更多还原