色谱

色谱 ›› 2019, Vol. 37 ›› Issue (5): 547-550.DOI: 10.3724/SP.J.1123.2018.11011

• 研究论文 • 上一篇    下一篇

气相色谱法测定阳离子表面活性剂合成体系中脂肪烷基二甲基叔胺

罗红元1,2, 秦飞3, 罗联忠1,2, 叶廷秀3, 刘平华3, 林雨桑3   

  1. 1. 厦门市海洋药用天然产物资源重点实验室, 厦门医学院, 福建 厦门 361023;
    2. 海洋生物医药资源福建省高校工程研究中心, 厦门医学院, 福建 厦门 361023;
    3. 厦门医学院药学系, 福建 厦门 361023
  • 收稿日期:2018-11-08 出版日期:2019-05-08 发布日期:2015-03-23
  • 通讯作者: 罗红元,E-mail:luohongyuan515@163.com
  • 基金资助:

    厦门市科技局计划项目（3502Z20163021）；厦门市海洋与渔业局产业技术专项（17GYY008NF04）.

Determination of fatty alkyl dimethyl tertiary amines by gas chromatography in the synthesis of cationic surfactants

LUO Hongyuan1,2, QIN Fei3, LUO Lianzhong1,2, YE Tingxiu3, LIU Pinghua3, LIN Yusang3   

  1. 1. Xiamen Key Laboratory of Marine Medicinal Natural Products Resources, Xiamen Medical College, Xiamen 361023, China;
    2. Engineering Center for Marine Biomedical Resource Utilization, Xiamen Medical College, Xiamen 361023, China;
    3. Department of Pharmacy, Xiamen Medical College, Xiamen 361023, China
  • Received:2018-11-08 Online:2019-05-08 Published:2015-03-23
  • Supported by:

    Science and Technology Project of Xiamen (No. 3502Z20163021); Scientific Research Project of Xiamen Southern Ocean Center (No. 17GYY008NF04).

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摘要：

选用HP-NINOWax毛细管色谱柱及氢火焰离子化检测器（FID），采用程序升温，建立了4种脂肪烷基二甲基叔胺的分析方法。结果表明，4种脂肪烷基二甲基叔胺质量浓度在0.005~1.0 g/L范围内，其峰面积与质量浓度有良好的线性关系，相关系数（R2）在0.9996以上。检出限（LODs，信噪比为3）在0.001~0.002 g/L之间，定量限（LOQs，信噪比为10）在0.003~0.005 g/L之间，回收率在90%~130%之间，相对标准偏差为1.3%~6.9%（n=6）。方法的线性范围宽、回收率高、选择性好，可用于叔胺的产品质量分析及生产过程控制分析。利用该方法对阳离子表面活性剂合成反应中十六烷基二甲基叔胺进行监测，结果很好地符合双分子亲核取代反应。该方法比滴定分析法更快速、精确，与液相色谱法相比，不需要进行柱前衍生或者使用色谱-质谱联用仪器。

关键词: 气相色谱, 阳离子表面活性剂, 脂肪烷基二甲基叔胺

Abstract:

A method to determine fatty alkyl dimethyl tertiary amines by gas chromatography (GC) was set up using HP-INNOWax capillary column, hydrogen flame ionization detector (FID) and temperature programming. The linearities were all excellent in the range of 0.005-1.0 g/L with the correlation coefficients being above 0.9996. The limits of detection (LODs, S/N=3) of the method were between 0.001 g/L and 0.002 g/L, and the limits of quantification (LOQs, S/N=10) were between 0.003 g/L and 0.005 g/L. The recoveries ranged between 90% and 130% with relative standard deviations of 1.3%-6.9% (n=6). The proposed method has the advantages of wide linear range, higher recovery, and selectivity, which was suitable for the quantitative analysis of fatty alkyl dimethyl tertiary amines and monitoring process control in industrial production. The method was faster and more accurate than titration, and also precluded the need for pre-column derivatization and determination by liquid chromatography-tandem mass spectrometry.

Key words: cationic surfactants, fatty alkyl dimethyl tertiary amines, gas chromatography (GC)

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