微波辅助萃取-气相色谱法同时测定皮革及其制品中21种有害有机溶剂残留量  

Simultaneous Determination of the Residual Contents of 21 Harmful Organic Solvents in Leather and Leather Products by Gas Chromatography Coupled with Microwave- assisted Extraction

作　　者：王成云[1] 施钦元[1] 邬晓慧[1] 林镱琳 沈雅蕾[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：《西部皮革》2015年第16期28-33,共6页West Leather

基　　金：国家质检总局科研项目(2012IK119;2014IK163)

摘　　要：建立了一个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方法。该方法以甲醇为萃取溶剂，85℃下微波辅助萃取皮革及其制品中残留的有害有机溶剂，萃取物经固相萃取柱净化后直接进行气相色谱分析，外标法定量。各组分的检出限为0.05-0.50ms／kg，在3个不同加标水平下，平均加标回收率为81．65％～95．84％，精密度实验RSD为1．76—4．18％（n=9）。该方法操作简单，灵敏度高，检出限低，能满足REACH法规的限量要求，可用于皮革及其制品中有害有机溶剂残留量的测定。An effective gas chromatographic method was established to determine simultaneously the residual contents of 21 harmful organic solvents in leather and leather products. Harmful organic solvents in leather and leather products were microwave - assisted extracted at 85℃, using methanol as the extraction solvent. The extract was first purified by solid -phase extraction （SPE） column, and then analyzed by gas chromatography - flame ionization detector （ GC - FID） technique. The concentration of each analyte was calibrated by the external standard method. The limits of detection （LODs） varied from 0. 05 mg/kg to 0. 50 mg/kg. The average recovery ratio changed from 81.65% to 95.84% under three different spiked levels while the relative standard deviation changed from 1.76% to 4. 18%. The proposed method was simple, accurate and sensitive, and the limits of detection （LOD） could meet the limited requirements of regulation concerning registration, evaluation, authorization and restriction of chemicals （REACH）. It was applicable to the determination of residual contents of harmful organic solvents in leather and leather products.

关 键 词：微波辅助萃取 气相色谱-火焰离子检测器 皮革 REACH法规 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]