气相色谱―质谱法测定仿真饰品中磷酸酯类增塑剂含量  

Determination of Phosphate Plasticizers in Imitation Jewelry by Gas Chromatography-Mass Spectrometry

作　　者：林睿[1] 赖莺[1] 葛秀秀[1] 黄宗平[1] 林海霞[1] 林伟靖[1] 黄龙[1] 

机构地区：[1]厦门出入境检验检疫局技术中心,福建厦门361026

出　　处：《广州化学》2012年第2期1-5,29,共6页Guangzhou Chemistry

基　　金：国家质检总局课题"仿真饰品中有毒有害物质的检测技术和风险分析研究"(2009IK075)

摘　　要：建立了仿真饰品中6种磷酸酯类增塑剂含量的气相色谱―质谱测定法。对提取方法、色谱条件及质谱参数进行了研究。结果表明,采用正己烷/丙酮(体积比1∶1)微波萃取样品35 min可获得良好的提取效果。所建立的微波萃取―气相色谱―质谱法的定量限为1～2.5 mg/kg,在1～2个数量级浓度范围内,线性相关系数R2在0.999以上,在三个添加水平下回收率在86.63%～98.13%之间。对市售9种塑料仿真饰品的测定结果表明磷酸酯的存在风险极低。A method was developed for the determination of 6 phosphate plasticizers in imitation jewelry by gas chromatography-mass spectrometry （GC-MS）. Extraction, chromatography and mass conditions were studied. Results showed that the extraction of target compounds can reach a good performance with hexane-ketone （1 ： l） under microwave assisted extraction for 35 rain. The limit of quantification （LOQ） of the method was 1-2.5 mg/kg. The calibration curves were linear within the concentration of 1-2 order of magnitude with typical correlation coefficients above 0.999. The recoveries ranged from 86.63%-98.13% with three addition levels. Risk of the presence of phosphate plasticizers in imitation jewelry was very low according to the results from 9 commercial samples.

关 键 词：仿真饰品 磷酸酯 微波萃取 气相色谱―质谱法 

分 类 号：O657.63[理学—分析化学]