A novel method was established to determine the alkyl and aromatic organophosphate esters fire retardant in textile by solid phase extraction (SPE) and GC-MS. Organophosphate esters fire retardant were extracted from textile with acetonitrile-toluene (3 : 1, V/V) mixture, then target analytes were purified by ENVI-Carb SPE column, and finally analyzed by GC-MS. The linear range of Tris(2,3-dibromopropyl) phosphate (TDBPP) was in the range of 0. 050 - 20. 0 mg/L with a correlation coefficient (r) of 0. 9859, and of other target analytes were in the range of 0. 010 - 20.0 mg/L with r ranging from 0. 9998 to 1. 000. The quantitation limit (S/N = 10) was 0.050 mg/kg for TDBPP, and 0. 010 mg/kg for other analytes. The feasibility of this method was demonstrated by determination of organophosphate esters fire retardant in textile samples with spiked recoveries, which was in the range between 71. 4% and 102. 5% (RSD ≤4. 9%, n=6). Among 20 samples analyzed, only one I typed sample was detected with tributylphosphate (TBP) concentration of (62. 2 + 0. 3) μg/kg.%建立了固相萃取-气质联用法同时测定纺织品中的烷基磷酸三酯和芳香基磷酸三酯类阻燃剂的方法.采用乙腈-甲苯(3∶1,Ⅴ/Ⅴ)混合溶液作为提取剂,对纺织品中的磷酸三酯类阻燃剂进行提取；再用ENVI-Carb固相萃取柱对提取液中的目标分析物进行净化处理；氮吹浓缩定容后,用气质联用仪进行定性与定量分析.磷酸三(2,3-二溴丙基)酯在0.050～20 mg/L浓度范围内存在良好的线性关系,相关系数r为0.9859;定量限为0.050 mg/kg (S/N=10).其它目标分析物在0.010～20 mg/L浓度范围内存在良好的线性关系,r为0.9998～1.000;定量限为0.010 mg/kg(S/N=10).本方法成功应用于纺织品中磷酸三酯类阻燃剂的检测,加标回收率在71.4％～102.5％之间；RSD≤4.9(n=6).分析的20个样品中,有一个Ⅰ类样品检出TBP,含量为(62.2±0.3) μg/kg.
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