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×0.10μm)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)。
In this study,a reliable gas chromatography-mass spectrometry method was developed for simultaneous deter-mination of five novel flame retardants,including 4-tert-butylphenyl diphenyl phosphate(MDPP),2-ethylhexyltetrabro-mobenzoate(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-assist-ed methanol extraction,followed by separation on a DB-5HT capillary column(15 m×0.25 mm×0.10μm)with tem-perature 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 concentra-tion 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 accura-cy and precision for analyzing these emerging contaminants in plastic matrices.
作者
李支薇
钱秀敏
张兰兰
林华珍
丁恩恩
秦宇媚
赖朝坤
LI Zhiwei;QIAN Xiumin;ZHANG Lanlan;LIN Huazhen;DING Enen;QIN Yumei;LAI Chaokun(GRG Metrology&Test Group Co,Ltd,Guangzhou 510700,China;CRRC Changchun Railway Vehicles Co,Ltd,Changchun 130062,China)
出处
《中国塑料》
北大核心
2025年第9期101-107,共7页
China Plastics
基金
广州市青年科技人才托举工程项目(QT20230101322)。
关键词
气相色谱质谱联用
再生塑料
新型阻燃剂
gas chromatography-mass spectrometry
recycled plastic
novel flame retardants
作者简介
通信作者: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。
