中国塑料 ›› 2025, Vol. 39 ›› Issue (9): 101-107.DOI: 10.19491/j.issn.1001-9278.2025.09.016

• 助剂 • 上一篇    

气相色谱质谱法测定再生塑料中5种新型阻燃剂

李支薇1, 钱秀敏2, 张兰兰1(), 林华珍1, 丁恩恩1, 秦宇媚1, 赖朝坤1   

  1. 1.广电计量检测集团股份有限公司,广州 510700
    2.中车长春轨道客车股份有限公司,长春 130062
  • 收稿日期:2024-10-14 出版日期:2025-09-26 发布日期:2025-09-22
  • 通讯作者: 张兰兰(1986-),女,高级工程师,研究方向:环保检测技术研究,zhangll2@grgtest.com
    E-mail:zhangll2@grgtest.com
  • 基金资助:
    广州市青年科技人才托举工程项目(QT20230101322)

Determination of novel flame retardants in recycled plastic by gas chromatography⁃mass spectrometry

LI Zhiwei1, QIAN Xiumin2, ZHANG Lanlan1(), LIN Huazhen1, DING Enen1, QIN Yumei1, LAI Chaokun1   

  1. 1.GRG Metrology & Test Group Co,Ltd,Guangzhou 510700,China
    2.CRRC Changchun Railway Vehicles Co,Ltd,Changchun 130062,China
  • Received:2024-10-14 Online:2025-09-26 Published:2025-09-22
  • Contact: ZHANG Lanlan E-mail:zhangll2@grgtest.com

摘要:

建立了一种测定再生塑料中磷酸叔丁基苯二苯酯(MDPP)、2⁃乙基己基⁃四溴苯甲酸(TBB)、磷酸苯基(二叔丁基苯基)酯(DBPP)、磷酸三(对⁃叔丁基苯)酯(TBPP)和2,3,4,5⁃四溴⁃苯二羧酸双(2⁃乙基己基)酯(TBPH)的气相色谱质谱(GC⁃MS)联用方法。样品经甲苯进行超声提取,采用升温程序在DB⁃5HT(15 m×0.25 mm×0.10 μm)毛细管色谱柱上对目标化合物进行分离,通过GC⁃MS的SCAN和SIM模式同时进行分析。结果表明,5种新型阻燃剂在浓度0.05~10 mg/L范围内具有良好的线性关系,相关系数r2均大于0.998;检出限和定量限分别为0.12~0.18 mg/kg及0.40~0.60 mg/kg;在3个浓度水平下的加标回收率在95.7 %~106.4 %之间,相对标准偏差在0.2 %~5.1 %之间(n=7)。

关键词: 气相色谱质谱联用, 再生塑料, 新型阻燃剂

Abstract:

In this study, a reliable gas chromatography⁃mass spectrometry method was developed for simultaneous determination of five novel flame retardants, including 4⁃tert⁃butylphenyl diphenyl phosphate (MDPP), 2⁃ethylhexyltetrabromobenzoate (TBB), bis(4⁃tert⁃butylphenyl)phenyl phosphate (DBPP), tris(p⁃t⁃butylphenyl)phosphate (TBPP), and bis(2⁃ethylhexyl)⁃2,3,4,5⁃tetrabromophthalate (TBPH), in recycled plastics. The method employed ultrasonic⁃assisted methanol extraction, followed by separation on a DB⁃5HT capillary column (15 m×0.25 mm×0.10 μm) with temperature programming. Identification and quantification were performed using both full scan and selected ion monitoring modes with external standard calibration. The method demonstrated excellent linearity (R²>0.998) across a concentration range of 0.05~10 mg/L. Method validation showed detection limits of 0.12~0.18 mg/kg and quantification limits of 0.40~0.60 mg/kg. Average recoveries at three spiking levels (0.5, 20 and 100 mg/kg) ranged from 95.7 % to 106.4 %, with relative standard deviations (RSDs, n=7) between 0.2 % and 5.1 %, confirming the method's accuracy and precision for analyzing these emerging contaminants in plastic matrices.

Key words: gas chromatography?mass spectrometry, recycled plastic, novel flame retardants

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