材料期刊网

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。

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. 0-15 312. 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.