微波辅助萃取-气质联用法同时测定皮革及其制品中21种有害有机溶剂的残留量  

Simultaneous Determination of the Residual Contents of 21 Harmful Organic Solvents in Leather and Leather Products by Gas Chromatography/Mass Spectrometry Combined with Microwave-assisted Extraction Technique

作　　者：王成云[1] 李心恬[1] 唐丽莉[1] 余侃[1] 杨怡然[1] 曾欣莉 

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 [2]深圳职业技术学院,广东深圳518055

出　　处：《西部皮革》2016年第3期30-36,共7页West Leather

基　　金：国家质检总局科研项目(2011IK105;2012IK119;2014IK163)

摘　　要：建立了一种同时测定皮革及其制品中21种有害有机溶剂残留量的气相色谱/质谱联用方法,该方法以甲醇为萃取溶剂,采用微波辅助萃取技术提取皮革及其制品中残留的有害有机溶剂,提取产物经固相萃取柱净化后,直接进行气质联用分析,外标法定量。21种有害有机溶剂的检出限为0.02-0.10 mg/kg,方法的加标平均回收率为82.4%-94.7%,相对标准偏差为1.7%-4.9%。该方法简单快速、灵敏度高、检出限低,可完全满足皮革及其制品中有害有机溶剂残留量检测工作的需要。应用该方法对市售皮革及其制品进行筛查,在部分样品中检出不同含量的多种目标分析物。An effective GC/MS method was established for the simultaneous determination of the residual contents of 21 kinds of harmful organic solvents in leather and leather products. Residual harmful organic solvents in leather and leather products were extracted using microwave-assisted extraction using methanol as the extraction solvent. The extracts were purified by a solid-phase extraction （SPE） column, and then analyzed by gas chromatography/mass spectrometry in selected ion monitoring mode （GC/MS-SIM）. The concentration of each target compound was calibrated by the external standard method. The limit of detection （LOD） of 21 hmrful organic solvents varied from 0.02 mg/kg to 0.10 mg/kg. The spiked average recoveries changed from 82.4% to 94.7% while the relative standard deviation （RSD） changed from 1.7% to 4.9%. This method was simple, rapid, sensitive and accurate, which could completely satisfy the technical demand on the determination of residual harmful organic solvents in leather and leather products. The proposed method was applied in the screening of residual harmful organic solvents in commercial leather and leather products and several target compounds at different content levels were detected in some samples.

关 键 词：微波辅助萃取 气质联用 皮革 有害有机溶剂 

分 类 号：TS262.4[轻工技术与工程—发酵工程]