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/Tandem Mass Spectrometry Coupled with Microwave-assisted Extraction

作　　者：王成云[1] 李心恬[1] 唐丽莉[1] 余侃[1] 杨怡然[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》2016年第1期5-11,共7页Leather And Chemicals

基　　金：国家质检总局科研项目(2012IK119;2014IK163)

摘　　要：建立了1个气相色谱，串联质谱方法，对皮革及其制品中21种有害有机溶剂的残留量进行了同时测定，该方法以甲醇为萃取溶剂，微波萃取皮革及其制品中残留的有害有机溶剂，萃取液经硅胶固相萃取柱净化后，直接进行气相色谱／串联质谱分析，外标法定量。结果表明，21种有害有机溶剂的定量下限为15～100μg/kg。在3个加标浓度水平下，方法的加标平均回收率为80．3～94．6％，相对标准偏差为2．5～7．3％。该方法简单快速。灵敏度高，定性准确，定量下限低，定量下限远低于欧盟REACH法规的限量要求，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中残留的有害有机溶剂含量进行筛查，结果在部分样品中检出了不同含量水平的多种目标分析物。An effective method was established to determine simultaneously the residual contents of 21 kinds of harmful organic solvents by gas chromatography-tandem mass spectrometry （GC/MS-MS） technique. Residual harmful organic solvents in leather and leather products were microwave-assisted extracted using methanol as the extraction solvent. The extract was then purified by a silica solid-phase extraction （SPE） column, followed by the analysis of gas chromatography/tandem mass Spectrometry （GC/MS-MS）. The concentration of each analyte was calibrated by external standard method. The limits of quantification （LOQs） of 21 harmful organic solvents varied from 15 μg/kg to 100 μg/kg. The spiked average recoveries varied from 80.3% to 94.6% while the relative standard deviation changed from 2.5% to 7.3% under three different spiked levels. The proposed method was simple, rapid, sensitive and accurate, and the limits of quantification （LOQs） far less the limited requirements of Regulation Concerning Registration, Evaluation, Authorization and Restriction of Chemicals （REACH） of European Union. It could satisfy completely the technical demand of 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 leather and leather products available commercially, and several target compounds at different content levels were detected in some samples.

关 键 词：微波辅助萃取 气相色谱 串联质谱 皮革 N-甲基吡咯烷酮 酰胺 乙二醇醚 

分 类 号：TS57[轻工技术与工程—皮革化学与工程] O657.63[理学—分析化学]