在线催化–气相色谱串联质谱法测定再生塑料原料中C_(14)~C_(17)氯化石蜡  

Determination of C_(14)-C_(17) chlorinated paraffins in recycled plastic raw material by online catalytic–gas chromatography tandem mass spectrometry

作　　者：张子豪 林海 李春燕 王晶 彭莹 余建龙 肖前 ZHANG Zihao;LIN Hai;LI Chunyan;WANG Jing;PENG Ying;YU Jianlong;XIAO Qian(Guangzhou Customs District Technology Center.,Guangzhou 510623,China;Zhanjiang Customs District Technology Center.,Zhanjiang 524000,China)

机构地区：[1]广州海关技术中心,广州510623 [2]湛江海关技术中心,广东湛江524000

出　　处：《化学分析计量》2022年第9期26-31,共6页Chemical Analysis And Meterage

基　　金：广州海关科研项目(2020GZCK-015,2022GZCK08)。

摘　　要：建立在线催化–气相色谱串联质谱技术对再生塑料原料中C_(14)~C_(17)氯化石蜡进行测定。样品经冷冻粉碎后,用正己烷萃取,以SPE固相萃取柱净化分离,采用装有催化衬管的气相色谱串联质谱仪进行测定,C_(14)~C_(17)氯化石蜡经催化脱氯加氢后转化为正构烷烃,经DB–5MS UI色谱柱(30 m×0.25 mm×0.25μm)分离,多反应监控模式测定,以内标法定量。还原产物C_(14)~C_(17)直链烷烃的质量浓度在20~1000 ng/mL范围内线性关系良好,相关系数不小于0.9955。C_(14)~C_(17)直链烷烃的方法定量限为0.007~0.018μg/mL,相当于样品中C_(14)~C_(17)的氯化石蜡总和为0.77μg/g。样品加标回收率为91.3%~104.1%,测定结果的相对标准偏差不大于5.77%(n=6)。该方法适用于再生塑料原料中C_(14)~C_(17)氯化石蜡含量的筛查和快速测定。A method for the determination of C_(14)-C_(17) chlorinated paraffins in recycled plastic raw material was established by online catalytic–gas chromatography tandem mass spectrometry.Samples were cryogenic grinding and extracted with n-hexane,purified and separated by solid phase extraction column,determined by gas chromatography tandem mass spectrometer with catalytic liner tube containing catalyst.After catalytic dechlorination and hydrogenation,C_(14)-C_(17) chlorinated paraffins were converted into n-alkanes,which were separated by DB–5MS UI(30 m×0.25 mm×0.25μm)column,determined by multiple reaction monitoring mode,quantified by internal standard method.The mass concentration of reduced products C_(14)-C_(17) linear alkanes had a good linear relationship in the range of 20–1000 ng/mL,and the correlation coefficient was not less than 0.9955.The limit of quantification of C_(14)-C_(17) linear alkane was 0.007–0.018μg/mL,which was equivalent to 0.77μg/g of C_(14)-C_(17) chlorinated paraffins in the sample.The recovery of spiked samples was 91.3%–104.1%,and the relative standard deviation of the determination results was not more than 5.77%(n=6).This method is suitable for screening and rapid determination of C_(14)-C_(17) chlorinated paraffins in imported recycled plastic raw materials.

关 键 词：再生塑料 串联质谱 C_(14)~C_(17)氯化石蜡 

分 类 号：O657[理学—分析化学]