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作 者:李宣[1] 杨曦[1] 麦宝华[1] 于文杰[1] 禹伟腾[1]
出 处:《分析测试学报》2013年第8期1020-1023,共4页Journal of Instrumental Analysis
基 金:国家质检总局科技计划项目(2009IK114);深圳出入境检验检疫局科技计划项目(SZ2011014)
摘 要:建立了气相色谱-质谱联用法定性和定量分析塑料中环己烷1,2-二甲酸二异壬酯(DINCH)的方法。考察了DINCH分子离子的质谱断裂过程,并建立了快速鉴定塑料中DINCH的理论方法。通过对不同溶剂提取效率的对比,采用二氯甲烷作为最佳提取溶剂。在优化条件下,该方法的线性范围为0.24~1.60 mg/L,相关系数为0.998,定量下限(S/N=10)为1.2 mg/kg。在加标水平为80~400 mg/kg时,4种不同塑料(PE、PP、PU、PVC)的回收率和相对标准偏差分别为82%~113%和1.1%~9.0%。将该方法用于实际塑料样品的检测,结果满意。A method was developed for the qualitative and quantitative analysis of DINCH in plastics by GC - MS. The key fragmentation processes of the mass spectrum were elucidated based on the mass spectrum theory, and the fragmentation experiment of these ions could provide theoretical knowledge for the rapid identification of the existence or not of DINCH in plastics. Based on the com parison of extraction efficiencies of different organic solvents, dichloromethane was used as extraction solvent in the method. The test result showed that the method had a good linear relationship (r = 0. 998)in the range of 0. 24 -1.60 mg/L. The limit of quantitation( LOQ, S/N= 10) was 1.2 mg/ kg. At spiked levels of 80 - 400 mg/kg in plastics ( PE, PP, PU, PVC ) , the average recoveries were in the range of 82% - 113% , with relative standard deviations of 1.1% -9. 0%. The method was applied in the determination of DINCH in plastics samples with satisfactory results.
关 键 词:环己烷1 2-二甲酸酯 质谱 裂解规律 气相色谱-质谱联用分析
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