超声萃取/气相色谱-质谱联用法测定汽车涂料中的11种芳香胺
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摘要
建立了气相色谱-质谱联用法(GC-MS)测定汽车涂料中的11种芳香胺的方法,以乙腈为溶剂,采用超声萃取前处理,高速离心,过滤取清液后,通过Elite-5MS色谱柱分离,质谱测定,选择离子监测模式定量。结果表明:11种芳香胺在0.6~30 mg/L范围内线性关系良好,相关系数大于0.997,定量限为0.25~2.36 mg/kg,检出限为0.08~0.73 mg/kg,加标回收率和精密度良好,加标回收率在86.2%~109.8%之间,精密度<6.9%。方法能够满足汽车涂料中11种芳香胺的分析要求。
A gas chromatography-mass spectrometry (GC-MS) method for the determination of 11 kinds of aromatic amines in automobile coatings was established.The samples were dissolved in acetonitrile and treated by ultrasonic extraction,centrifuged at high speed and filtered.The filtrate was separated by Elite-5 MS column and identified by mass spectrometry.The analytes were quantified by the selected ion monitoring mode.The results showed that the linear ranges of 11 kinds of aromatic amines were from 0.6 to 30 mg/L,with correlation coefficients greater than 0.997.The limits of quantification and detection were from 0.25 to 2.36 mg/kg and 0.08 to 0.73 mg/kg,respectively.And the recoveries ranged from 86.2% to 109.8%,with relative standard deviations less than 6.9%.The method can be used to determine the 11 kinds of aromatic amines in automobile coatings.
A gas chromatography-mass spectrometry (GC-MS) method for the determination of 11 kinds of aromatic amines in automobile coatings was established.The samples were dissolved in acetonitrile and treated by ultrasonic extraction,centrifuged at high speed and filtered.The filtrate was separated by Elite-5 MS column and identified by mass spectrometry.The analytes were quantified by the selected ion monitoring mode.The results showed that the linear ranges of 11 kinds of aromatic amines were from 0.6 to 30 mg/L,with correlation coefficients greater than 0.997.The limits of quantification and detection were from 0.25 to 2.36 mg/kg and 0.08 to 0.73 mg/kg,respectively.And the recoveries ranged from 86.2% to 109.8%,with relative standard deviations less than 6.9%.The method can be used to determine the 11 kinds of aromatic amines in automobile coatings.
引文
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[5]Lei F M,Du C,Li J.China Fib Insp,2013,33(14):74雷发懋,杜潮,李进.中国纤检,2013,33(14):74
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[12]Gu H,Qin X,Hu J L.Chin J Anal Lab,2014,33(02):236顾虎,秦鑫,胡建兰.分析试验室,2014,33(02):236