微波辅助萃取-气相色谱质谱法测定聚合物中9种有机磷酸酯化合物  

Determination of 9 organophosphorus esters in polymer by microwave-assisted extraction and gas chromatography-mass spectrometry

作　　者：林殷[1] 杜凤娟[2] 王璨[1] 林鹏辉[1] 

机构地区：[1]汕头出入境检验检疫局检验检疫技术中心,汕头515041 [2]广东检验检疫技术中心,广州510625

出　　处：《分析试验室》2017年第2期226-230,共5页Chinese Journal of Analysis Laboratory

摘　　要：建立了一种同时检测聚合物材料中9种有机磷酸酯化合物(OPEs)的分析方法。通过萃取溶剂选择实验和正交实验,确定了以15 m L丙酮为萃取溶剂,萃取温度110℃,萃取时间10 min的微波萃取条件。聚合物样品中的OPEs经微波萃取后,采用气相色谱-质谱联用法(GC-MS)进行分析。结果表明,该方法中9种OPEs的线性相关系数为0.9994~0.9999,检出限为0.2~1.9 mg/kg,空白样品加标回收率为86.5%~106.0%,相对标准偏差(RSD)为1.6%~8.6%。本方法样品适用性较为广泛、通用性强,适用于聚合物材料中多种OPEs的同时检测。A determination method for 9 organophosphorus esters（OPEs） in polymer materials was developed.The orthogonal and solvent selection experiments were designed to optimize the microwaveassisted extraction conditions.The OPEs in samples were extracted by microwave-assisted extraction using 15 mL of acetone under the conditions of 110℃ for 10 min and detected by gas chromatographymass spectrometry（GC-MS）.The results showed that the correlation coefficients,limits of detection（LOD）,recoveries and relative standard deviations（RSDs） are 0.9994 - 0.9999,0.2 - 1.9 mg/kg,86.5% - 106.0%,and 1.6% - 8.6%,respectively.This method has advantages of wide application range and universality,and can be applied for the simultaneous determination of various OPEs.

关 键 词：有机磷酸酯化合物 微波辅助萃取 气相色谱-质谱联用法 聚合物材料 

分 类 号：TQ075[化学工程]