微波辅助萃取-气相色谱/质谱-选择离子监测法同时测定皮革制品中21种邻苯二甲酸酯类化合物  

Simultaneous determination of 21 kinds of phthalates in leather products by gas chromatography/mass spectrometry-selected ion monitor technique coupled with microwave-assisted extraction

作　　者：王成云[1] 岑杨媚[1] 麦家超[1] 沈雅蕾[1] 谢堂堂[1] 刘彩明[1] 

机构地区：[1]深圳出入境检验检疫局,深圳518045

出　　处：《分析仪器》2012年第6期29-35,共7页Analytical Instrumentation

摘　　要：建立了气相色谱/质谱-选择离子监测方法,对皮革制品中21种邻苯二甲酸酯类化合物进行了同时测定。该方法以乙腈为萃取溶剂,对皮革制品进行微波辅助萃取,萃取物经中性氧化铝固相萃取柱净化处理后进行气相色谱/质谱-选择离子监测法测定。该方法快速简便,定性定量准确,检出限低,DIDP和DINP的检出限分别为2.0、1.0mg/kg,其余各组分的检出限均低于0.4mg/kg。该方法的精密度试验的RSD均小于9%,加标平均回收率为88.75～97.86%。采用该方法对47个市售皮革制品进行测定,结果在2个样品中检出多种邻苯二甲酸酯类化合物。An effective GS/MS-SIM method was established to determine simultaneously the contents of 21 kinds of phthalates in leather products. Phthalates in leather products were micro-wave-assisted extracted using acetonitrile as the extraction solvent, then the extracts were puri-fied by neutral alumina solid extraction column, followed by the analysis applying gas chromatography/mass spectrometry-selected ion monitor （GC/MS-SIM） technique. The proposed method was rapid, accurate, and sensitive. The detection limits of DIDP and DIDN were 2.0mg/kg and 1.0mg/kg, respectively. The detection limits of other phthalates were all less than 0.4mg/kg. The relative standard deviation （RSD） of precision experiment was all less than 9M. The spiked average recoveries changed from 88.75 % to 97.86%. The proposed method was applied successfully to determine the contents of phthalates in 47 commercially available leather products and phthalates were found to exist in two samples.

关 键 词：皮革制品 气相色谱 质谱-选择离子监测法 邻苯二甲酸酯 微波辅助萃取 

分 类 号：O657.63[理学—分析化学] TS57[理学—化学]