微波萃取/GC-MS法测定塑料制品中的六溴环十二烷

建立了采用微波萃取/气相色谱-质谱(GC-MS)法检测塑料制品中六溴环十二烷的方法。将破碎后的样品用正己烷/丙酮(1:1)混合溶剂进行微波萃取,萃取液经硅胶小柱净化、平行蒸发定量浓缩后采用GC-MS法测定含量,外标法定量。优化了样品前处理条件,包括前处理方式的选择、微波萃取溶剂和萃取时间的选择,以及净化小柱的选择。对于六溴环十二烷标准溶液,在50~1000mg/L范围内,线性关系良好,相关系数大于0.999;方法定量测定下限为100mg/kg,相对标准偏差为2.1%~5.8%,加标回收率为81.3%~104%。该方法操作简便分、析迅速结、果准确可,以满足对塑料产品中六溴环十二烷的定性和定量分析。

Determination of Hexabromocyclododecane in Plastic Products by Microwave Extraction/GC-MS Method

A new method was established for the determination of hexabromocyclododecane (HBCD) in plastic products by microwave extraction technique combining with GC-MS method. The sample was crushed and then extracted with hexane/acetone (1:1) mixed solvent in microwave extraction equipment at 80 ℃ for 2 h. The extract was purified with silica gel solid phase extraction cartridge, and then quantitatively concentrated with parallel evaporation instrument. The pretreatment condition, including the extraction method, extractant, microwave extraction time and SPE cartridge was optimized. Under the optimum separation and detection condition, HBCD were confirmed and determined with external standard method. The standard curves of HBCD solution were linear in the concentration range of 50~1 000 mg/L with correlation coefficient more than 0.999. The recoveries ranged from 81.3% to 104%,with the relative standard deviation(RSD) of 2.1%~5.8%. The lower limit of determination (LDL) was 100 mg/kg. This method was rapid, simple, accurate, and was suitable for qualitatively confirm and quantitatively analysis of the content of HBCD in plastic products.