Fast, very fast, and ultra-fast gas chromatography-mass spectrometry of thermally labile steroids, carbamates, and drugs in supersonic molecular beams
Fast, very fast, and ultra-fast gas chromatography-mass spectrometry of thermally labile steroids, carbamates, and drugs in supersonic molecular beams
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在超声分子束中对热不稳定类固醇、氨基甲酸酯和药物进行快速、极快和超快速气相色谱-质谱分析
DOI：
10.1016/1044-0305(96)80519-8
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发表时间：
1996
影响因子：
3.2
通讯作者：
A. Amirav
中科院分区：
文献类型：
--
作者：
S. Dagan;A. Amirav
采用短柱快速气相色谱仪，结合超音速分子束中的飞通电子电离，研究了热不稳定化合物的气相色谱-质谱分析方法。对32种化合物进行了分析，其中包括类固醇、氨基甲酸酯类、农药、抗生素药物和其他药物化合物，并提供了其GC-MS分析的详细信息。分析热不稳定化合物的能力与分析速度有关。定义了一个新的术语“速度增强因子”（SEF），即与常规GC-MS条件相比，柱长减少与载气线速度增加的乘积。快速、极快速和超快速GC-MS的SEF范围分别为5-30、30-400和400-4000。在解离程度，速度，气相色谱仪分辨率和灵敏度的权衡进行了研究，并检查了热不稳定的分子。描述了影响解离的实验因素，重点是解离的还原。我们声称使用超音速分子束进行采样和电离为热不稳定化合物的GC-MS提供了最终的能力。得到了70 ev的电子电离质谱，表明分子离子的相对丰度增强，质谱库检索能力强，优于粒子束液相色谱-质谱法。比较了超声分子束快速气相色谱-质谱法与其他快速气相色谱-质谱法及粒子束液相色谱-质谱法的性能。
Gas chromatography-mass spectrometry (GC-MS) analyses of thermally labile compounds have been studied by using a short column fast gas chromatograph, coupled with fly-through electron ionization in supersonic molecular beams. Thirty-two compounds, which include steroids, carbamate pesticides, antibiotic drugs, and other pharmaceutical compounds, have been analyzed and the details of their GC-MS analysis are provided. The ability to analyze thermally labile compounds is discussed in relation to the speed of analysis. A new term, “speed enhancement factor” (SEF), is defined as the product of column length reduction and the carrier gas linear velocity increase, as compared with normal GC-MS conditions. Fast, very fast, and ultra-fast GC-MS are defined with a SEF in the ranges of 5–30, 30–400, and 400–4000, respectively. Trade-offs in the degree of dissociation, speed, gas chromatograph resolution, and sensitivity were studied and examined with thermally labile molecules. The experimental factors that affect the dissociation are described with emphasis on its reduction. We claim that the use of supersonic molecular beams for sampling and ionization provides the ultimate capability in the GC-MS of thermally labile compounds. The obtained 70-eV electron ionization mass spectra are shown, and an enhanced relative abundance of the molecular ion is demonstrated together with library search capability of these mass spectra, which is better than that reported with particle beam liquid chromatography-mass spectrometry. The performance of fast GC-MS in supersonic molecular beams is compared with other methods of fast GC-MS and with particle beam liquid chromatography-mass spectrometry.