纺织品中禁用有机磷阻燃剂的超声萃取-气相色谱/质谱-选择离子监测法测定

Determination of Organophosphorous Flame Retardants in Textiles by Gas Chromatography/Mass Spectrometry after Ultrasonic Extraction

建立了同时测定纺织品中6种禁用有机磷阻燃剂的气相色谱/质谱-选择离子监测(GC/MS-SIM)方法。以丙酮为萃取溶剂,超声萃取纺织品中禁用有机磷阻燃剂,萃取液进行气相色谱/质谱-选择离子监测法测定。6种禁用有机磷阻燃剂三-(1-氮杂环丙基)氧化膦(TEPA)、三-(2-氯乙基)磷酸酯(TCEP)、三-(1,3-二氯丙基)磷酸酯(TDCP)、二-(2,3-二溴丙基)磷酸酯(DDBPP)、三-(邻甲苯基)磷酸酯(TOCP)和三-(2,3-溴丙基)磷酸酯(TRIS)的定量限(S/N=10)分别为0.020、0.001、0.005、1.000、0.003、0.500mg/kg。方法的精密度为4.16%～8.79%,回收率为85.12%～94.71%。采用该方法对市售纺织品进行测试,结果在部分样品中检出高浓度的TCEP、TDCP及TOCP。

An analytical method was established for the simultaneous determination of six organophosphorous flame retardants in textiles. Organophosphorous flame retardants in textiles were ultrasonically extracted using acetone as the extraction solvent, and then were analyzed by gas chromatography-mass spectrometry with selected ion monitor technique. The limits of quantification were 0. 020,0. 001,0. 005, 1. 000,0. 003 and 0. 500 mg/kg for TEPA,TCEP, TDCP,DDBPP, TOCP and TRIS,respectively, at the condition of signal to noise（S/N） = 10. The recoveries for the spiked samples varied from 85. 12% to 94.71% while the relative standard deviation（RSD） ranging from 4.16%to 8.79%. Organophosphorous flame retardants in commercially available textiles were detected and the result showed that TCEP, TDCP and TOCP existed at high content in some flame retardant textiles.