气相色谱串联质谱法测定塑料玩具中14种非邻苯二甲酸酯类增塑剂  

Determination of 14 non-phthalates plasticizers in plastic toys by gas chromatography-tandem mass spectrometry

作　　者：杨倩 冉露 何小玲 余秋玲 邱月 陆嘉莉 YANG Qian;RAN Lu;HE Xiaoling;YU Qiuling;QIU Yue;LU Jiali(Chongqing Academy of Metrology and Quality Inspection,Chongqing 401123,China)

机构地区：[1]重庆市计量质量检测研究院,重庆401123

出　　处：《分析试验室》2024年第11期1563-1570,共8页Chinese Journal of Analysis Laboratory

基　　金：重庆市科技局科研院所绩效激励引导专项(cstc2022jxjl50001);重庆市市场监督管理局科研计划项目(CQSJKJ2022040);重庆市市场监督管理局科研计划项目(CQSJKJ2021041)资助。

摘　　要：基于气相色谱串联质谱法(GC-MS/MS)建立了同时测定聚氯乙烯(PVC)和丙烯腈-丁二烯-苯乙烯(ABS)塑料玩具中14种非邻苯二甲酸酯类增塑剂的检测方法。剪碎后的玩具样品经乙酸乙酯于60℃超声提取40 min,过0.45μm聚四氟乙烯(PTFE)滤膜,目标物经TG-5Sil MS色谱柱分离,在电子轰击源(EI)下进行选择反应监测(SRM)测定,外标法定量。分别对仪器条件和前处理条件进行了优化,同时对基质干扰和基质效应进行了考察。结果表明,GC-MS/MS抗干扰能力强,样品提取液无需净化直接测定;基质效应对分析结果的影响可忽略不计。在0.01~2.00 mg/L线性范围内,14种非邻苯二甲酸酯类增塑剂的相关系数(R^(2))均大于0.995,检出限(LOD)为0.13~0.50 mg/kg,平均加标回收率为88.8%~112.1%,相对标准偏差(RSD)为1.6%~7.9%。对市售30批次玩具样品进行检测,检出8种非邻苯二甲酸酯类增塑剂,其中对苯二甲酸二辛酯(DOTP)的检出率高达63.3%,最高检出浓度达2.0×10^(5) mg/kg。该方法适用于塑料玩具中14种非邻苯二甲酸酯类增塑剂的检测。A method for the simultaneous determination of 14 non-phthalate plasticizers (non-PAEs) in polyvinyl chloride (PVC) and acrylonitrile-butadiene-styrene (ABS) plastic toys was developed by gas chromatographytandem mass spectrometry (GC-MS/MS).The shredded plastic toy samples were extracted by ultrasonic extraction with ethyl acetate at 60℃for 40 min,and filtered through 0.45μm polytetrafluoroethylene (PTFE) membrane.The target compounds were separated by TG-5Sil MS column,and then determined by selective reaction monitoring (SRM) mode under electron bombardment source (EI),and quantified by external standard method.The instrument conditions and pre-treatment conditions were optimized respectively.The matrix interferences and matrix effects were investigated.The results showed that GC-MS/MS had strong antiinterference ability,and the sample extract was directly measured without purification.The influence of matrix effects on the analysis results could be ignored.The correlation coefficients (R^(2)) of 14 non-PAEs were all above 0.995 in the linear ranges of 0.01-2.00 mg/L,the limits of detection (LODs) were 0.13-0.50 mg/kg,the average recoveries were 88.8%-112.1%,and the relative standard deviations (RSDs) were 1.6%-7.9%.The 8 non-PAEs were detected in 30 batches of commercial toys.The highest detection rate of dioctyl terephthalate (DOTP) was 63.3%,and the highest detection concentration of DOTP was 2.0×10~5 mg/kg.This method is suitable for the determination of 14 non-PAEs in plastic toys.

关 键 词：气相色谱-串联质谱法 塑料玩具 非邻苯二甲酸酯类增塑剂 

分 类 号：O657.63[理学—分析化学]