微波辅助萃取/气相色谱-质谱联用法同时测定皮革及其制品中12种乙二醇醚类有机溶剂残留量  

Simultaneous Determination of Residual Contents of 12 Glycol Ethers in Leather and Its Products by Gas Chromatography-Mass Spectrometry Coupled with Microwave-assisted Extraction

作　　者：王成云[1] 张伟亚[1] 李丽霞[1] 唐莉纯[1] 林君峰[1] 沈雅蕾[1] 黄明珠[1] 谢堂堂[1] 褚乃清[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：《分析测试学报》2014年第12期1380-1386,共7页Journal of Instrumental Analysis

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：以甲醇为溶剂,85℃下微波萃取皮革及其制品中的乙二醇醚类有机溶剂,萃取物经固相萃取柱净化后进行气相色谱-质谱/选择离子监测法测定,外标法定量,从而建立了同时测定皮革及其制品中12种乙二醇醚类有机溶剂残留量的气相色谱-质谱联用方法.该方法的加标回收率为81.1％ ～ 95.9％,相对标准偏差（RSD,n=9）为1.4％ ～9.6％.在信噪比（S/N）为10的条件下,各组分的定量下限（LOQ）为0.05 ～0.20mg/kg.该方法操作简单、方便快速、灵敏度高,可满足皮革及其制品中乙二醇醚类有机溶剂残留量检测的技术要求,并为制定相关检测标准提供了参考.An effective method was established for the simultaneous determination of the residual contents of 12 glycol ethers in leather and its products.Glycol ethers in leather and leather products were microwave-assisted extracted at 85 ℃,using methanol as extraction solvent.The extracts were purified with solid phase extraction （SPE） column,and analyzed by gas chromatography-mass spectrometry/selected ions monitoring technique （GC-MS/SIM） with the external standard method.The spiked average recoveries varied from 81.1％ to 95.9％ with relative standard deviations（RSDs） of 1.4％-9.6％.The limits of quantitation （LOQ,S/N =10） for analytes were in the range of 0.05-0.20 mg/kg.The proposed method was simple,rapid,sensitive and accurate,and could satisfy completely the technical demands for the determination of glycol ethers residual in leather and its products and provide a reference for the relevant testing standard.

关 键 词：微波辅助萃取 皮革 气相色谱-质谱法 乙二醇醚 

分 类 号：O657.63[理学—分析化学] TQ413.2[理学—化学]