| 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 |
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| 基金项目:国家质检总局科研项目（2011IK105,2012IK119,2014IK163） |
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| 中文摘要: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。 |
| 中文关键词: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 |
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| Determination of Residues of 21 Harmful Organic Solvents in Leather and Leather Products by Gas Chromatography-Mass Spectrometry Combined with Ultrasonic Extraction |
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| Abstract: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 50μg/kg for ethylene glycol dibutyl ether（EGDBE）,triethylene glycol dimethyl ether（TEGDME）,diethylene glycol butyl ether（DEGBE） and triethylene glycol ethyl ether（TEGEE）,150μg/kg for N-methylformamide（MF） and N-methylacetamide（MA）,300μg/kg for formamide,and 100μg/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. |
| Key Words:ultrasonic extraction gas chromatography-mass spectrometry（GC-MS） selected ion monitoring（SIM） leather glycol ethers amides N-methylpyrrolidone |
| 引用本文：王成云*，施钦元，褚乃清，林君峰，谢堂堂.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[J].分析测试学报,2016,35(4):380-387. |
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