微波萃取/GC-MS法对电子电气产品中多氯萘的测定

建立了微波萃取/GC-MS法检测电子电气产品中多氯萘的方法。将破碎后的样品以甲苯为溶剂进行微波萃取,萃取液经硅胶小柱净化、平行蒸发定量浓缩后采用气相色谱-质谱法测定多氯萘的含量,外标法定量。优化了样品前处理条件,包括前处理方式、微波萃取溶剂、萃取时间,以及净化小柱的选择。对于8种含不同氯原子数的多氯萘,在1~50 mg/L范围内,线性关系良好,相关系数均大于0.995;方法定量下限为0.2~1.0 mg/kg,相对标准偏差为2.7%~7.2%,回收率为77%~112%。该法操作简便、分析迅速、结果准确,可以满足对电子电气产品中多氯萘的定性确证和定量分析。

Determination of Polychlorinated Naphthalenes in Electrical and Electronic Products by Microwave Extraction and GC-MS Method

A new method was established for the determination of polychlorinated naphthalenes(PCNs) in electrical and electronic products by microwave extraction technique combining with GC-MS method.The sample was crushed and then extracted with toluene in microwave extraction equipment at 120 ℃ for 2 hours.The extract was purified with silica gel solid phase extraction cartridge, and then quantitatively concentrated with parallel evaporation instrument.The pretreatment conditions, including extraction method, extractant, microwave extraction time and SPE cartridge were optimized.Under the optimum separation and detection condition, PCNs were confirmed and determined with external standard method.The standard curves of 8 PCNs with different chlorine atoms were linear in the concentration range of 1-50 mg/L with correlation coefficients of more than 0.995.The recoveries ranged from 77% to 112%,with the relative standard deviations(RSDs) of 2.7% -7.2%.The limit of quantitation(LOQs) were in the range of 0.2-1.0 mg/kg.This method was rapid, simple, accurate, and was suitable for qualitatively confirm and quantitatively analysis the content of PCNs in electrical and electronic products.