Assay of High-carbon Dialkyl Carbonates by HPLC-MS in Hyphenation
摘 要
采用高效液相色谱与质谱联用技术,可使由低碳酸酯与碳数超过10的高碳醇反应所得产物碳酸高碳二烷基酯达到良好的分离、分析以及结构鉴定.在色谱分析中采用Novapak C18(3.9 mm×150 mm)色谱柱及无水乙醇作流动相并用示差检测器检测.质谱离子源采用大气压化学电离源(APCI).试验表明:此法适用于碳酸高碳二烷基酯合成过程的监测和产品的质量控制.
Abstract
By the application of high performance liquid chromatography and mass spectrometry in hyphenation,satisfactory separation and assaying as well as structural identification of the main reaction product,dialkyl carbonate,produced by the reaction between low carbon alkyl carbonate and high carbon alcohol with carbon number greater than 10,was attained.The Novapak C18 column (3.9 mm×150 mm) column was used as stationary phase and absolute alcohol was used as mobile phase in chromatography with differential detector.The ion source used in mass spectrometry was the APCI.It was proved that the proposed method was feasible for supervision and control of product-quality of the process of synthesis of high-carbon dialkyl carbonates.
中图分类号 O657.63
所属栏目 工作简报
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收稿日期 2009/5/5
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备注李进(1964-),男,陕西西安人,高级工程师,长期从事润滑油添加剂分析工作.
引用该论文: LI Jin,LI Li-xia,CHENG Wei. Assay of High-carbon Dialkyl Carbonates by HPLC-MS in Hyphenation[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(11): 1330~1331
李进,李丽霞,程伟. 高效液相色谱-质谱联用法分析碳酸高碳二烷基酯[J]. 理化检验-化学分册, 2010, 46(11): 1330~1331
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【3】覃玲,罗光毅,陈海珍.微波消解-双道原子荧光光谱法同时测定水产品中砷和汞[J].微量元素与健康研究,2009,26(1):48-49.
【4】李波,崔杰华,刘东波,等.微波消解-氢化物发生原子荧光法同时测定土壤中的砷汞[J].分析试验室,2008,27(7):601,701.
【5】黄先飞,秦樊鑫,胡继伟,等.微波消解-原子荧光法测定头花蓼中痕量砷[J].时珍国医国药,2008,19(3):577-579.
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