微波辅助萃取-气相色谱法同时测定皮革及其制品中乙二醇醚类有机溶剂的残留量  

Simultaneous Determination of Residual Glycol Ethers in Leather and Leather Products by Gas Chromatography Coupled with Microwave-assisted Extraction

作　　者：王成云[1] 唐莉纯[1] 李丽霞[1] 钟声扬[1] 李燕华[1] 林君峰[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：《皮革与化工》2014年第4期30-36,共7页Leather And Chemicals

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

摘　　要：建立了一个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方法，该方法以甲醇为萃取溶剂，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-火焰离子化检测器（GC-FID）测定，外标法定量。该方法的加标平均回收率为81.21%-98.16%，相对标准偏差（RSD）为1.36%-4.87%。在信噪比（S/N）=3的条件下，各组分的检出限为0.05-0.30 mg/kg，远远低于REACH法规的限量要求。该方法操作简便，方便快速，检测通量大，灵敏度高，可完全满足皮革及其制品中乙二醇醚类有机溶剂检测的技术要求，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 residual glycol ethers in leather and leather products by gas chromatography-flame ionization detector （GC-FID） technique, coupled with microwave assisted extraction. Glycol ethers in leather and leather products were microwave-assisted extracted at 85℃, using methanol as the extraction solvent. The extracts were then purified by solid phase extraction （SPE） column, followed by the analysis of gas chromatography-flame ionization detector （GC-FID）. The contents of each analyte were calibrated by external standard method. The limits of detection （LODs） varied from 0.05mg/kg to 0.30mg/kg at the condition of signal to noise （S/N） of 3, far less than the limited requirements of Regulation Concerning Registration, Evaluation, Authorization and Restriction of Chemicals （REACH） of European Union. The spiked average recoveries changed from 81.21%to 98.16%while the relative standard deviation （RSD） varied＆amp;nbsp;from 1.36%to 4.87%. The proposed method was simple, rapid and sensitive, and completely met the technical demands of the determination of glycol ethers in leather and leather products. The proposed method provided a reference for the relevant testing standard.

关 键 词：微波辅助萃取 皮革 气相色谱- 火焰离子化检测器法 乙二醇醚类 

分 类 号：O657.71[理学—分析化学] TS57[理学—化学]