超声萃取-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 GC-MS/MS Coupled with Ultrasonic Extraction

作　　者：王成云[1] 李丽霞[1] 谢堂堂[1] 林君峰[1] 褚乃清[1] 唐莉纯[1] 李燕华[1] 

机构地区：[1]深圳出入境检验检疫局,广东深圳518045

出　　处：《质谱学报》2016年第2期121-133,共13页Journal of Chinese Mass Spectrometry Society

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

摘　　要：为监控皮革及其制品中有害有机溶剂的残留量,建立了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-串联质谱（GC-MS/MS）法。以乙酸乙酯为萃取溶剂,超声萃取皮革及其制品中残留的有害有机溶剂,萃取液经固相萃取柱净化后进行GC-MS/MS分析,外标法定量。结果表明,各组分的检出限为15～100μg/kg,平均加标回收率为80.6%～95.8%,精密度（RSD）为2.3%～6.7%（n=9）。采用该方法测定512个市售皮革制品中21种有机溶剂的残留量,在其中的55个样品中检出N,N-二甲基甲酰胺（DMF）、N,N-二甲基乙酰胺（DMA）、乙二醇单乙醚（EGEE）、乙二醇单丁醚（EGBE）、二乙二醇单乙醚（DEGEE）、二乙二醇单丁醚（DEGBE）、三乙二醇单甲醚（TEGME）、三乙二醇单丁醚（TEGBE）、N-甲基吡咯烷酮（NMP）等9种目标分析物,其中检出率最高的是DEGBE和DMF,检出含量最高的是DEGBE。该方法快速简便、灵敏度高,适用于皮革及其制品中有害有机溶剂残留量的检测。In order to monitor the residual contents of harmful organic solvents in leather and leather products,a method of gas chromatography-tandem mass spectrometry（GC/MS-MS）was established for the simultaneous determination of 21 harmful organic solvents.Residual harmful organic solvents in leather and leather products were ultrasonically extracted using ethyl acetate as the extraction solvent,then the extract waspurified by solid-phase extraction（SPE）column and was analyzed by GC-MS/MS.All the analyte were calibrated by the external method.The results show that the limits of quantification（LOQ）are 15μg/kg for ethylene glycol diethyl ether（EGEE）,ethylene glycol dibutyl ether（EGDBE）and N-methylpyrrolidone（NMP）;the limit of quantification is 20μg/kg for ethylene glycol methyl ether（EGME）;the limits of quantification are 25μg/kg for diethylene glycol dimethyl ether（DEGDME）, N,N-dimethylformamide（DMF）,ethylene glycol butyl ether（EGBE）,N,N-dimethylacetamide（DMA）,N-methylformamide（MF）and diethylene glycol butyl ether（DEGBE）;the limits of quantification are 50μg/kg for ethylene glycol dimethyl ether（EGDME）,ethylene glycol ethyl ether（EGEE）,diethylene glycol methyl ether（DEGME）,diethylene glycol ethyl ether（DEGEE）,N-methylacetamide（MA）,triethylene glycol dimethyl ether（TEGDME）,formamide,triethylene glycol methyl ether（TEGME）,triethylene glycol ethyl ether（TEGEE）and triethylene glycol butyl ether（TEGBE）;the limit of quantification is 100μg/kg for diethylene glycol diethyl ether（DEGDEE）.The spiked average recoveries are 80.6%-95.8% under three different spiked levels.The relative standard deviation（RSD）of precision experiment changes from 2.3%to 6.7%.By using this method,512 commercially available leather and leather product samples were detected and 9target compounds such as DMF,DMA,EGEE,EGBE,DEGEE,DEGBE,TEGME,TEGBE and NMP were found to exist in 55 samples.The ratios of detection of DEGBE and DMF are the highest among these 9ta

关 键 词：气相色谱-串联质谱法(GC-MS/MS) 皮革制品 超声萃取 酰胺 乙二醇醚 N-甲基吡咯烷酮 

分 类 号：O657.63[理学—分析化学]