超声萃取-GC-MS测定皮革及制品中溶剂残留——15种乙二醇醚同时测定  

15 Glycol Ethers Residues Simultaneous Determination in Leather and Leather Products by Ultra. Extracting-GC-MS

作　　者：王成云[1] 褚乃清[1] 张伟亚[1] 谢堂堂[1] 林君峰[1] 李丽霞[1] 

机构地区：[1]深圳出入境检验检疫局工业品检测技术中心,广东深圳518067

出　　处：《皮革科学与工程》2015年第4期66-73,共8页Leather Science and Engineering

基　　金：国家质检总局科研项目(2011IK105;2012IK119);国家认监委科研制标项目(2013B239k)

摘　　要：以乙酸乙酯为萃取溶剂,45℃下超声萃取皮革及其制品中残留的乙二醇醚类有机溶剂,萃取产物经固相萃取柱净化后,进行气相色谱/串联质谱分析,外标法定量,从而建立了一个同时测定皮革及其制品中15种乙二醇醚类有机溶剂残留量的气质联用方法。在信噪比（S/N）=10的条件下,各组分的定量下限为5-20 g/kg,方法的平均加标回收率为80.60%-91.48%,相对标准偏差为3.20-6.94%。该方法简便快速,定量下限远远低于相关标准的限量要求,可满足皮革及其制品中乙二醇醚类有机溶剂残留量检测工作的需要,为制定相关检测标准提供了参考。A method was established for the simultaneous determination of the residues of 15 glycol ethers in leather and leather products by gas chromatography/tandem mass spectrometry. Residual glycol ethers in leather and leather products were ultrasonically extracted at 45 ℃ using ethyl acetate as the extraction solvent. The extracts were then purified by solid phase extraction（SPE） column, followed by gas chromatography/tandem mass spectrometric analysis. The concentration of each analyte was calibrated by external standard method. The limits of quantification（LOQs） varied from 5 g/kg to 20 g/kg at the condition of signal to noise（S/N） of 10. The spiked average recoveries changed from 80.60% to 91.48% while the relative standard deviation（RSD） varied from 3.20% to 6.94%. The proposed method was simple, rapid and accurate, and the LOQs far less than the limited requirements of relevant regulations. It could satisfy completely the technical demands of the determination of glycol ethers in leather and leather products and provided a reference for the relevant testing method.

关 键 词：气相色谱/串联质谱法 乙二醇醚类 超声萃取 皮革 

分 类 号：TS57[轻工技术与工程—皮革化学与工程] O658.2[理学—分析化学]