中国塑料 ›› 2023, Vol. 37 ›› Issue (10): 8-14.DOI: 10.19491/j.issn.1001-9278.2023.10.002

• 材料与性能 • 上一篇    下一篇

GC⁃MS/MS法检测聚氨酯泡沫塑料中14种有机磷酸酯阻燃剂

余敏()   

  1. 南平市产品质量检验所,福建 南平,353000
  • 收稿日期:2023-07-23 出版日期:2023-10-26 发布日期:2023-10-23
  • 作者简介:余敏(1969-),男,高级工程师,从事检验质量、检测方法研究,190451635@qq.com
  • 基金资助:
    福建省市场监督管理局《关于印发2018年第四批福建省地方标准制修订计划项目的通知》(闽质监 [2018] 263号)

Determination of 14 organophosphate ester flame retardants in polyurethane foam through GC⁃MS/MS

YU Min()   

  1. Quality Inspection Institute of Nanping,Nanping 353000,China
  • Received:2023-07-23 Online:2023-10-26 Published:2023-10-23

摘要:

基于气相色谱⁃串联质谱法(GC⁃MS/MS),建立了聚氨酯泡沫塑料中14种有机磷酸酯阻燃剂残留的检测方法,采用丙酮超声提取并浓缩,再经定容过滤后用气相色谱⁃串联质谱测定,外标法定量。通过参数优化,结果表明,磷酸三(2⁃氯乙基)酯(TCEP)和磷酸三间甲苯酯(TMCP)在0.02~0.2 mg/L、磷酸三(丁氧基乙基)酯(TBEP)在0.05~0.5 mg/L、其余11种有机磷酸酯在0.01~0.1 mg/L梯度浓度内具有良好线性关系(线性相关系数>0.995),TCEP和TMCP的定量限为0.33 mg/kg,检出限为0.10 mg/kg;TBEP的定量限为0.83 mg/kg,检出限为0.25 mg/kg;其余11种有机磷酸酯的定量限为0.17 mg/kg,检出限为0.05 mg/kg。三梯度加标平行试验加标回收率介于87.0 %~108.1 %之间,相对标准偏差介于2.5 %~10.6 %之间。

关键词: 聚氨酯泡沫, 有机磷酸酯阻燃剂, 超声提取, 气相色谱?串联质谱

Abstract:

Based on gas chromatography⁃tandem mass spectrometry (GC⁃MS/MS), a detection method for 14 types of organic phosphate flame retardants in polyurethane foams was established through adopting ultrasonic extraction and concentration with acetone, filtering with a constant volume, determining with gas chromatography⁃tandem mass spectrometry, and quantifying with an external standard method. Through parameter optimization, the experimental results indicated that there was a good linear relationship at gradient concentrations of tris(2⁃chloroethyl) phosphate (TCEP) and Tri⁃m⁃cresylphosphate (TMCP) in the range of 0.02~0.2 mg/L, a gradient concentration of tris(2⁃butoxyethyl) phosphate (TBEP) in the range of 0.05~0.5 mg/L, and gradient concentrations of the remaining 11 organic phosphates in the range of 0.01~0.1 mg/L with a linear correlation coefficient greater than 0.995. In this case, the quantification limit of TCEP and TMCP was 0.33 mg/kg, and their limit of detection was 0.10 mg/kg. The quantification limit of TBEP was 0.83 mg/kg, and its limit of detection was 0.25 mg/kg. The quantification limit of the ester was 0.17 mg/kg, and its limit detection was 0.05 mg/kg. The recoveries of three gradient spiked parallel experiments ranged from 87.0 % to 108.1 %, and their relative standard deviations ranged from 2.5 % to 10.6 %.

Key words: polyurethane foam, organophosphate flame retardant, ultrasonic extraction, gas chromatography?tandem mass spectrometry

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