基于热解分离-气相色谱-串联质谱技术测定聚合物再生原料中得克隆类衍生物  

Determination of Dechlorane Plus Derivatives in Recycled Polymer Material by Pyrolysis-Gas Chromatography-Tandem Mass Spectrometry

作　　者：张子豪 霍炜江 王晶 肖前 刘莹峰 李全忠 郑建国 ZHANG Zi-hao;HUO Wei-jiang;WANG Jing;XIAO Qian;LIU Ying-feng;LI Quan-zhong;ZHENG Jian-guo(Guangzhou Customs District Technology Center,Guangzhou 510623,China)

机构地区：[1]广州海关技术中心,广东广州510623

出　　处：《分析测试学报》2024年第8期1265-1272,共8页Journal of Instrumental Analysis

基　　金：国家重点研发计划(2022YFF0607201);广州海关科研项目(2022GZCK08、2022GZCK11);广州市科技计划项目(2023A04J0700)。

摘　　要：采用分步热解分离-气相色谱-串联质谱(EGA-GC-MS/MS)建立了快速测定固体聚合物再生原料(再生纸浆、再生塑料)中6种新发的得克隆类衍生物的方法。样品预先切割成小块,在裂解仪中程序加热升温,使得克隆类衍生物于聚合物裂解前气化析出,以ZB-5HT石英毛细管柱为分离柱,在多反应监测(MRM)模式下使用内标法进行质谱测定。对热解分离条件、色谱和质谱条件进行了优化,在最佳实验条件下,6种得克隆类衍生物在10.0~500μg/g范围内具有良好的线性关系,定量下限为4.5~11.4 mg/kg。再生纸浆的加标回收率为85.3%~113%,相对标准偏差(RSD,n=6)不大于6.4%;再生塑料聚合物的加标回收率为86.2%~116%,RSD(n=6)不大于7.2%。该方法无需冷冻粉碎、萃取等步骤,可直接进样分析,具有操作简便快速、灵敏度高等优点,适用于固体聚合物再生原料中得克隆类衍生物的测定。A method for determination of dechlorane plus derivatives in solid polymer recycled mate⁃rials(recycled pulp,recycled plastics)was established by stepwise pyrolysis-gas chromatographytandem mass spectrometry(EGA-GC-MS/MS).Sample were cut up in advance and heated in the py⁃rolysis furnace.6 dechloraneplus derivatives were evolving before polymer pyrolysis.The dechlorane⁃plus derivatives were separated by ZB-5HT INFERNO column,and analyzed using tandem mass spectrometry employing the internal standard method and multi-reaction monitoring mode(MRM).In this paper,pyrolysis and chromatography-mass spectrometry conditions were optimized.Under the optimized experimental conditions,a linear correlation of 6 dechlorane plus derivatives was observed between 10.0-500μg/g,and quantitation limits were 4.5-11.4 mg/kg.Recycling pulp samples yielded recoveries ranging from 85.3%-113%,with relative standard deviations(RSDs)not higher than 6.4%.Recoveries of plastic polymer samples were 86.2%-116%with their RSDs(n=6)not high⁃er than 7.2%.The sample can be directly injected for analysis without pre-treatment such as freezing,grinding and extraction.This method is simple,rapid and sensitive,which is suitable for qualitative analysis and determination of dechlorane plus derivatives from solid polymer regenerated raw materials.

关 键 词：再生塑料 再生纸浆 得克隆类衍生物 逸出气体分析 气相色谱-串联质谱 

分 类 号：O657.7[理学—分析化学] X132[理学—化学]