超声萃取/气相色谱-质谱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  

Determination of Residues of 21 Harmful Organic Solvents in Leather and Leather Products by Gas Chromatography-Mass Spectrometry Combined with Ultrasonic Extraction

作　　者：王成云[1] 施钦元[1] 褚乃清[1] 林君峰[1] 谢堂堂[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：《分析测试学报》2016年第4期380-387,共8页Journal of Instrumental Analysis

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

摘　　要：建立了气相色谱-质谱/选择离子监测方法,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。该方法以乙酸乙酯为萃取溶剂,45℃下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气相色谱-质谱/选择离子监测法分析,外标法定量。结果表明,在信噪比（S/N）为10的条件下,乙二醇二丁醚（EGDBE）、三乙二醇二甲醚（TEGDME）、二乙二醇单丁醚（DEGBE）和三乙二醇单乙醚（TEGEE）的定量下限均为50μg/kg,N-甲基乙酰胺（MA）和N-甲基甲酰胺（MF）的定量下限均为150μg/kg,甲酰胺的定量下限为300μg/kg,其余14种组分的定量下限均为100μg/kg。在3个不同加标水平下,方法的平均加标回收率为82.1%-94.9%,相对标准偏差（RSD,n=9）为1.6%-4.8%。该方法简单快捷,灵敏度高,可用于皮革及其制品中有害有机溶剂残留量的测定。A method was established to determine simultaneously the residues of 21 harmful organic solvents in leather and leather products by gas chromatography-mass spectrometry in selected ion monitoring mode（GC-MS / SIM）.Residual harmful organic solvents in leather and leather products were ultrasonically extracted at 45 ℃,using ethyl acetate as extraction solvent.The extracts were purified with solid-phase extraction（SPE） columns,and then analyzed by gas chromatography-mass spectrometry in selected ion monitoring mode（GC-MS / SIM）.The content of each analyte was calibrated by the external standard method.At the condition of signal to niose（S / N） of ten,the limits of quantitation（LOQs） were 50 μg / kg for ethylene glycol dibutyl ether（EGDBE）,triethylene glycol dimethyl ether（TEGDME）,diethylene glycol butyl ether（DEGBE） and triethylene glycol ethyl ether（TEGEE）,150 μg /kg for N-methylformamide（MF） and N-methylacetamide（MA）,300 μg /kg for formamide,and 100 μg / kg for all the other fourteen compounds.The spiked average recoveries varied from 82.1% to 94.9% at three spiked levels with relative standard deviations（RSD） of 1.6%-4.8%.The proposed method was simple,rapid,accurate and sensitive,and was suitable for the determination of residual harmful organic solvents in leather and leather products.

关 键 词：超声萃取 气相色谱-质谱 选择离子监测 皮革 乙二醇醚 酰胺 N-甲基吡咯烷酮 

分 类 号：O657.63[理学—分析化学] TQ413.2[理学—化学]