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以丙酮为萃取溶剂,建立了超声波辅助萃取、气相色谱-质谱法(GC-MS)测定皮革中阻燃剂磷酸三(2-氯乙基)酯含量的方法。考察了6种不同萃取溶剂对磷酸三(2-氯乙基)酯的萃取效率,选择了丙酮为最佳萃取溶剂,考察了超声波辅助萃取温度与时间对萃取效果的影响,确定了最佳的超声波辅助萃取条件。萃取液经浓缩后,用气相色谱-质谱仪进行的定性及定量分析。结果表明:该方法的检出限为0.04mg/kg,样品的加标回收率在86.5%~96.8%之间,重复测量结果之间的相对标准偏差小于4.4%。该方法简便快速、灵敏度高、重复性好,可用于皮革制品中磷酸三(2-氯乙基)酯的检测。
A method for the determination of tris (2-chloroethyl) phosphate in leather by ultrasonic-assisted extraction and gas chromatography-mass spectrometry (GC-MS) was established using acetone as the extraction solvent. The extraction efficiency of tris (2-chloroethyl) phosphate with six different extraction solvents was investigated. Acetone was selected as the optimal extraction solvent. The effects of ultrasonic-assisted extraction temperature and time on the extraction efficiency were investigated. The best Ultrasonic-assisted extraction conditions. The extracts were concentrated and analyzed qualitatively and quantitatively by gas chromatography-mass spectrometry. The results showed that the detection limit of this method was 0.04 mg / kg, the recoveries of spiked samples ranged from 86.5% to 96.8%, and the relative standard deviations of repeated measurements were less than 4.4%. The method is simple, rapid, sensitive and repeatability and can be used for the determination of tris (2-chloroethyl) phosphate in leather products.