气相色谱法测定纺织品中的三种有机磷阻燃剂

Determination of Three Organophosphorous Flame Retardants in Textiles by Gas Chromatography

建立了超声萃取-毛细管气相色谱-氮磷检测器测定纺织品中3种有机磷阻燃剂的方法。正交试验确定超声萃取的优化条件为萃取溶剂丙酮和正己烷的体积比为2：8，萃取时间为40min，溶剂体积为35mL。实验结果表明，三（2-氯乙基）磷酸酯、三邻甲苯基磷酸酯和三（2，3-二溴丙基）磷酸酯等3种化合物的线性范围分别为0．3758～36．38mg／L、0．3841～38．41mg／L和15．78～1010mg／L，检测限依次为0．044，0．053和0．82mg／kg。对于上述3种化合物，方法的精密度分别为6．2％，7．7％和6．5％，方法的回收率介于83．2％和115．4％之间。

A method of simultaneous determination of three organophosphorous flame retardants in textiles by capillary gas chromatograph （GC） combined with nitrogen phosphorus detector （NPD） was developed. The samples were extracted by ultrasonic extraction, filtered by 0.22 um microporous film and then directly analyzed by GC-NPD. The ultrasonic extraction key factors optimized by the orthogonal design were as follows： the volume ratio of acetone to nhexane was 2： 8, the extraction time was 40 min and the solvent volume was 35 mL. The linear ranges of tris （2-chloroethyl） phosphate （TCEP）, tri-o-cresyl phosphate （TOCP） and tris （2,3-dibromopropyl） phosphate （TRIS） were 0. 375 8 - 36.38 ug/mL, 0. 384 1 - 38.41 ug/mL and 15.78 - 1 010 ug/mL, respectively, and the detection limits were 0. 044 mg/kg, 0. 053 mg/kg and 0.82 mg/kg, respectively. Textile samples including cotton, flax, nylon, silk and terylene spiked with different levels of the three flame retardants were employed to investigate the method precision and recovery. For aforementioned analytes, the method precisions were 6.2%, 7.7% and 6.5%, respectively and the method recoveries based on spiked studies were in the range of 83.2% - 115.4%. The method is suitable for the determination of three organophosphorous flame retardant residues in textiles in commodity inspection.