色谱 ›› 2015, Vol. 33 ›› Issue (1): 52-57.DOI: 10.3724/SP.J.1123.2014.07040

• 研究论文 • 上一篇    下一篇

气相色谱-质谱联用分析5种有机磷农药时氢气代替氦气作为载气的可行性考察

刘振学, 周仕学   

  1. 山东科技大学化学与环境工程学院, 山东 青岛 266590
  • 收稿日期:2014-07-23 修回日期:2014-09-24 出版日期:2015-01-08 发布日期:2014-12-26
  • 通讯作者: 刘振学
  • 基金资助:

    国家自然科学基金项目(21176145/B060901).

Feasibility investigation of hydrogen instead of helium as carrier gas in the determination of five organophosphorus pesticides by gas chromatography-mass spectrometry

LIU Zhenxue, ZHOU Shixue   

  1. College of Chemical & Environment Engineering, Shandong University of Science & Technology, Qingdao 266590, China
  • Received:2014-07-23 Revised:2014-09-24 Online:2015-01-08 Published:2014-12-26

摘要:

迄今为止,氦气几乎是气相色谱-质谱联用仪运行中唯一可选的载气.本文使用气相色谱-质谱联用仪考察了氢气和氦气分别作为载气时,对5种有机磷农药混合标准溶液的检测,以确定氢气代替氦气作为气相色谱-质谱联用仪载气用于有机磷农药分析的可行性.用工作站自带解卷积软件(自动质谱解卷积鉴定系统,AMDIS32),结合自建"有机农药质谱库"对结果进行了解析,而后用SPSS统计软件对数据进行了聚类分析.结果发现,以氢气为载气时虽然出峰稍快,但色谱峰分离度较低,解良度较低,且待测物信号不稳定,测定准确度较低,有些化合物甚至检测不到.因此以氢气为载气分析有机磷农药时应对测定准确度、信号稳定性、安全性等诸多因素进行慎重考虑.

关键词: 解良度, 气相色谱-质谱, 氢气, 有机磷农药, 载气, 自动质谱解卷积鉴定系统

Abstract:

Helium is almost the only choosable carrier gas used in gas chromatography-mass spectrometry (GC-MS). A mixed standard solution of five organophosphorus pesticides was analyzed by using GC-MS, and hydrogen or helium as carrier gas, so as to study the feasibility of hydrogen instead of helium as carrier gas for the determination of organophosphorus pesticides. Combining a mass spectrum database built by ourselves, the results were deconvolved and identified by Automated Mass Spectral Deconvolution & Identification System (AMDIS32), a software belonging to the workstation of the instrument. Then, the statistical software, IBM SPSS Statistics 19.0 was used for the clustering analysis of the data. The results indicated that when hydrogen was used as carrier gas, the peaks of the pesticides detected were slightly earlier than those when helium used as carrier gas, but the resolutions of the chromatographic peaks were lower, and the fraction good indices (Frac. Good) were lower, too. When hydrogen was used as carrier gas, the signals of the pesticides were unstable, the measuring accuracies of the pesticides were reduced too, and even more, some compounds were undetectable. Therefore, considering the measuring accuracy, the signal stability, and the safety, etc., hydrogen should be cautiously used as carrier gas in the determination of organophosphorus pesticides by GC-MS.

Key words: Automated Mass Spectral Deconvolution &, carrier gas, fraction good, gas chromatography-mass spectrometry (GC-MS), hydrogen, Identification System (AMDIS), organophosphorus pesticides

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