色谱

色谱 ›› 2015, Vol. 33 ›› Issue (11): 1186-1191.DOI: 10.3724/SP.J.1123.2015.05019

• 研究论文 • 上一篇    下一篇

固相萃取-气相色谱/质谱联用法测定儿童手推车中3种有机磷酸酯阻燃剂

赖晓芳, 冯岸红, 幸苑娜, 叶淋泉, 林志惠, 陈泽勇   

  1. 深圳市计量质量检测研究院, 广东 深圳 518131
  • 收稿日期:2015-05-13 出版日期:2015-11-08 发布日期:2012-05-30
  • 通讯作者: 冯岸红

Determination of three organophosphate ester flame retardants in baby carriages by gas chromatography-mass spectrometry combined with solid phase extraction

LAI Xiaofang, FENG Anhong, XING Yuanna, YE Linquan, LIN Zhihui, CHEN Zeyong   

  1. Shenzhen Academy of Metrology and Quality Inspection, Shenzhen 518131, China
  • Received:2015-05-13 Online:2015-11-08 Published:2012-05-30

PDF

149

被引次数

7

摘要：

有机磷酸酯是一类重要的磷系阻燃剂,由于其具有类似持久性有机污染物(persistent organic pollutants, POPs)的性质,欧美等国家已纷纷设立相关法规限制其在儿童用品中的使用。目前国际和国内均未有儿童手推车中有机磷酸酯阻燃剂的检测标准。本文建立了儿童手推车中3种有机磷酸酯阻燃剂的超声萃取-弗罗里硅土固相萃取柱净化-气相色谱/质谱检测方法。该方法的加标回收率为89.5%~107.3%,检出限(3S/N)为0.01 mg/kg,定量限(10S/N)为0.1 mg/kg,能较好地排除基质干扰,适用于儿童手推车软垫材料中3种有机磷酸酯的定性和定量分析。37个样品的分析结果表明,磷酸三(2-氯丙基)酯(TCPP)的检出率为81.1%,含量范围为1.0~15312.8 mg/kg,依据欧盟玩具新指令2014/79/EU, TCPP超标(> 5 mg/kg)率为32.4%;其中2个样品中还检出了磷酸三(2-氯乙基)酯(TCEP)和磷酸三(1,3-二氯-2-丙基)酯(TDCP),含量范围为6.2~44.1 mg/kg,均已超标。可见,市场上的儿童手推车存在较高的有机磷酸酯阻燃剂暴露风险。

关键词: 儿童手推车, 固相萃取, 气相色谱/质谱法, 有机磷酸酯阻燃剂

Abstract:

Organophosphate esters (OPEs) are high-production-volume chemicals used as flame retardants. Some western countries (e. g. America and European Union) have imposed restrictions on OPEs in baby products due to their similar persistent-organic-pollutants (POPs) properties. So far, there is no domestic or foreign standard for OPEs flame retardants in baby carriages. Ultrasonic extraction was used to extract three OPEs from baby carriages, and the extracts were purified by a florisil solid phase extraction (SPE) column, and finally detected by gas chromatography-mass spectrometry (GC-MS). The spiked recoveries of the three OPEs were in the range of 89.5% to 107.3%. The limits of detection (3S/N) were 0.01 mg/kg, and the limits of quantification (10S/N) were 0.1 mg/kg. This method could eliminate matrix effects and give accurate qualitative analytical results for the three OPE flame retardants in baby carriages. Thirty-seven samples were analyzed and the tris(2-chloro-1-methylethyl) phosphate (TCPP) detection rate was up to 81.1% with the mass concentration range of 1.0-15312.8 mg/kg, and 32.4% of the samples exceeded the European Union directive(2014/79/EU)for TCPP(> 5 mg/kg), as well as tris(2-chloroethyl) phosphate (TCEP) and tris[2-chloro-1-(chloromethyl)ethyl]phosphate(TDCP) in two samples, which were in the range of 6.2-44.1 mg/kg. Thus, relatively high OPEs flame retardants risk was presented in baby carriages.

Key words: baby carriages, gas chromatography-mass spectrometry (GC-MS), organophosphate ester (OPE) flame retardants, solid phase extraction (SPE)

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