色谱

色谱 ›› 2015, Vol. 33 ›› Issue (2): 146-151.DOI: 10.3724/SP.J.1123.2014.09051

• 研究论文 • 上一篇    下一篇

气相色谱-四极杆高分辨飞行时间质谱分析复杂芳烃体系中的苯甲醛、苯甲醇、苯乙酮与苯乙醛

刘俊彦1, 曹喆2, 李继文1, 汪哲明1, 王川1, 顾松园1   

  1. 1. 中国石化上海石油化工研究院, 上海 201208;
    2. 安捷伦科技(中国)有限公司, 上海 200233
  • 收稿日期:2014-10-08 修回日期:2014-10-30 出版日期:2015-02-08 发布日期:2015-01-24
  • 通讯作者: 刘俊彦

Application of gas chromatography-high resolution quadrupole time of flight mass spectrometry to the analysis of benzaldehyde, benzyl alcohol, acetophenone and phenylacetaldehyde in complex aromatic samples

LIU Junyan1, CAO Zhe2, LI Jiwen1, WANG Zheming1, WANG Chuan1, GU Songyuan1   

  1. 1. Sinopec Shanghai Research Institute of Petrochemical Technology, Shanghai 201208, China;
    2. Agilent Technologies, Shanghai 200233, China
  • Received:2014-10-08 Revised:2014-10-30 Online:2015-02-08 Published:2015-01-24

PDF

296

摘要：

建立了气相色谱-四极杆高分辨飞行时间串联质谱分析复杂芳烃体系样品中苯甲醛、苯甲醇、苯乙酮与苯乙醛的方法。该方法通过使用高分辨质谱得到目标化合物特征离子的精确质量数,结合色谱保留时间,有效排除了复杂芳烃体系样品本底中碎片离子的干扰,提高了定性与定量分析的准确性。使用目标化合物特征离子的质谱峰面积作为定量计算依据。苯甲醛、苯甲醇、苯乙酮与苯乙醛在各自的质量浓度范围内呈现良好的线性响应,回收率为87.97%~103.01%,定量限分别为0.04、0.10、0.08与0.03 mg/L,检出限分别为0.01、0.03、0.02与0.01 mg/L。对3份实际样品中的苯甲醛、苯甲醇、苯乙酮与苯乙醛进行了定量分析。本研究为气相色谱-四极杆高分辨飞行时间质谱技术应用于复杂体系中的微量杂质分析提供了一种新的思路和手段。通过精确的质量分辨和测定可以降低对色谱分离的依赖,弥补传统气相色谱-四极杆低分辨质谱技术的不足。

关键词: 复杂芳烃产物, 高分辨飞行时间质谱, 含氧化合物, 气相色谱

Abstract:

The study focuses on the quantitative analytical characterization of benzaldehyde, benzyl alcohol, acetophenone and phenylacetaldehyde in complex aromatic samples by gas chromatography-high resolution quadrupole time of flight mass spectrometry (GC-QTOF MS). The four compounds in real sample were accurately qualified and quantified through a comprehensive analysis of the GC retention times and the accurate masses of the ion fragments obtained by the high resolution MS. The new method therefore effectively avoids the interference of the real sample substrate, which reduces the accuracy of the analysis results. The peak area of the characteristic ion fragment for each compound was used for quantitation calculation. The MS signal responses of the four compounds showed good linear relationships with the corresponding mass concentrations and the linear regression coefficients were greater than 0.99. The method recoveries were 87.97%-103.01%. The limits of detection (LODs) were 0.01, 0.03, 0.02 and 0.01 mg/L for benzaldehyde, benzyl alcohol, acetophenone and phenylacetaldehyde respectively. The contents of the four compounds in three real samples were analyzed. The study provided a new strategy for oxygenate analysis in complex aromatic samples using GC-QTOF MS. By measuring the accurate masses, the new method reduces the reliance on chromatographic separation ability and makes up the shortcomings of the traditional GC-MS methods.

Key words: complex aromatic samples, gas chromatography (GC), high resolution time of flight mass spectrometry (HR TOF MS), oxygenates

中图分类号: