微波辅助萃取-气相色谱/串联质谱法同时测定皮革及其制品中15种乙二醇醚类有机溶剂的残留量  

Simultaneous Determination of the Residual Contents of 15 Glycol Ethers in Leather and Leather Products by Gas Chromatography/Tandem Mass Spectrometry Coupled with Microwave-assisted Extaction

作　　者：王成云[1] 张其芳[1] 林君峰[1] 沈雅蕾[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6期11-17,共7页Leather And Chemicals

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：以甲醇为萃取溶剂，85℃下微波辅助萃取皮革及其制品中残留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/串联质谱法分析，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3个加标水平下，该方法的加标平均回收率为81.30%~92.52%，相对标准偏差为2.91%~6.93%（n=9）。在信噪比（S/N）=10的条件下，各组分的定量下限为5~20 g/kg。该方法操作简单，快速准确，定量下限低，可完全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。采用该方法对市售皮革制品进行检测，在部分样品中检出不同含量水平的乙二醇醚类有机溶剂。An effective method was established to determine simultaneously the residual contents of 15 glycol ethers in leather and leather products. Residual glycol ethers in leather and leather products were microwave-assisted extracted at 85℃, using methanol as the extraction solvent. Then the extracts were purified by solid phase extraction column, followed by the analysis of gas chromatography/tandem mass spectrometry technique. The concentration of each analyte was calibrated by external standard method. The spiked average recoveries varied from 81.30% to 92.52% under three different spiked levels while the relative standard deviation （RSD） changed from 2.91% to 6.93%. The limits of quantification （LOQ） changed from 5 g/kg to 20 g/kg at the condition of signal to noise （S/N） of 10. The proposed method was simple, rapid, accurate and sensitive. It could satisfy completely the technical＆amp;nbsp;demands of the determination of residual glycol ethers in leather and leather products. The proposed method was applied in the determination of residual glycol ethers in commercially available leather and leather products and glycol ethers of different content levels were detected in some samples.

关 键 词：皮革 微波辅助萃取 气相色谱/串联质谱法 乙二醇醚 

分 类 号：O657.63[理学—分析化学] TS57[理学—化学]