高效液相色谱-氢化物发生原子荧光法同时测定塑料制品中的3种有机锡

Simultaneous Determination of Three Organotin Compounds in Plastic Products by High Performance Liquid Chromatography-Hydride Generation-Atomic Fluorescence Spectrometry

建立了高效液相色谱-氢化物发生原子荧光法联用同时测定塑料制品中二甲基锡、三甲基锡和二苯基锡的分析方法,优化了各实验参数.采用Agela-C18反相柱,流动相为甲醇-水-醋酸-三乙胺（60∶40∶1∶0.03）,流速为0.7 mL· min-1时,二甲基锡、三甲基锡和二苯基锡可达到基线分离.在5％ HCl和2％ KBH4的氢化反应条件下,二甲基锡、三甲基锡和二苯基锡混标溶液在10～200 μg·L-1浓度范围内均呈良好线性,其相关系数（r）均大于0.992.不同材质塑料样品经四氢呋喃溶解,甲醇沉淀杂质大分子高速离心过滤后,直接采用高效液相色谱-氢化物发生原子荧光法进行检测.测得PVC,PC,PS,AS,ABS不同塑料样品中二甲基锡、三甲基锡和二苯基锡的回收率为75.1％～109.1％,相对标准偏差为3.7％ ～ 10.7％,检出限分别为0.009,0.012,0.025 mg/kg.

A method based on high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry （HPLC-HG-AFS） for simultaneous determination of organotin compounds,e.g.dimethyltin（DMT）,trimethyltin （TMT） and diphenyltin （DPhT） in plastic samples was established.Various experimental parameters were optimized.DMT,TMT and DPhT were chromatographically separated on an Agela-C18 column by using mobile phase of methanol-water-acetic acid-triethylamine （60 ∶ 40 ∶ 1 ∶ 0.03） at a flow rate of 0.7 mL · min-1 The hydrogenation of organotin compounds reacted in the environment of 5％ HCl and 2％ KBH4.The different concentration mixed organotin compounds（DMT,TMT and DPhT） standard were tested.The experimental results indicated that the calibration curves were linear in the range of 10-200 μg/L with correlation coefficients （r） more than 0.992.Different plastic samples were dissolved completely in tetrahydrofuran（THF）,the impurities of high molecular weight were deposited by mixing methanol in THF solutions.The solutions were tested by HPLC-HG-AFS after high speed centrifugation and filtration.The average recoveries of DMT,TMT and DPhT in PVC,PC,PS,AS and ABS samples ranged from 75.1％ to 109.1％,with relative standard deviations of 3.7％-10.7％.The detection limits of DMT,TMT and DPhT were 0.009,0.012 mg/kg and 0.025 mg/kg,respectively.