Integrated gas chromatography-mass spectrometry

1973 ◽  
Vol 6 (3) ◽  
pp. 311-335 ◽  
Author(s):  
Ragnar Ryhage

Mass spectrometric analysis of organic compounds was in the early 1950s done mostly for quantitative determination of petroleum products. The use of the mass spectrometer for qualitative analysis of solid organic material samples was shown by O'Neil & Wier (1951) and since then a continuous increase in mass spectrometric studies of different classes of organic compounds has been noted. After the gas chromatograph was developed by James & Martin (1952) the quantitative analysis of complex mixtures of organic compounds was possible and after a few years the gas chromatographic method was considered as routine. The first connection of a gas chromatograph (GC) to a mass spectrometer (MS) was made by Holmes & Morell (1957). They studied gases using a splitter system where only a small part or less than 1% of the effluent from a packed column was transferred to the ion source of the mass spectrometer. The next step in GC—MS development was made by Gohlke (1959), who studied compounds of low molecular weight using capillary column directly connected to a time-of-flight mass spectrometer. This was possible due to the fact that the carrier gas flow rate could be limited to about 1 ml/min. To avoid the sample loss resulting from using a packed column with the splitter system a jet molecular separator was constructed as an interphase between the packed column and a mass spectrometer with magnetic sector analyser (Ryhage, 1964). Mixtures of fatty acids and of hydrocarbons with a molecular weight of up to about 420 were studied. In this study spectra were taken at irregular intervals.

2013 ◽  
Vol 34 (12) ◽  
pp. 3659-3664 ◽  
Author(s):  
Sehwan Park ◽  
Jihyeon Lee ◽  
Soo Gyeong Cho ◽  
Eun Mee Goh ◽  
Sungman Lee ◽  
...  

Molecules ◽  
2021 ◽  
Vol 26 (22) ◽  
pp. 6760
Author(s):  
De-Yi Huang ◽  
Meng-Jiy Wang ◽  
Jih-Jen Wu ◽  
Yu-Chie Chen

Atmospheric pressure chemical ionization (APCI)-mass spectrometry (MS) and electrospray ionization (ESI)-MS can cover the analysis of analytes from low to high polarities. Thus, an ion source that possesses these two ionization functions is useful. Atmospheric surface-assisted ionization (ASAI), which can be used to ionize polar and nonpolar analytes in vapor, liquid, and solid forms, was demonstrated in this study. The ionization of analytes through APCI or ESI was induced from the surface of a metal substrate such as a titanium slab. ASAI is a contactless approach operated at atmospheric pressure. No electric contacts nor any voltages were required to be applied on the metal substrate during ionization. When placing samples with high vapor pressure in condensed phase underneath a titanium slab close to the inlet of the mass spectrometer, analytes can be readily ionized and detected by the mass spectrometer. Furthermore, a sample droplet (~2 μL) containing high-polarity analytes, including polar organics and biomolecules, was ionized using the titanium slab. One titanium slab is sufficient to induce the ionization of analytes occurring in front of a mass spectrometer applied with a high voltage. Moreover, this ionization method can be used to detect high volatile or polar analytes through APCI-like or ESI-like processes, respectively.


1985 ◽  
Vol 31 (5) ◽  
pp. 741-746 ◽  
Author(s):  
D G Deutsch ◽  
R J Bergert

Abstract We evaluated the Hewlett-Packard 5995B benchtop capillary gas chromatograph-mass spectrometer (GC-MS) for its ability to identify drugs commonly detected and (or) measured in the clinical toxicology laboratory. Initial experiments indicated that the instrument as originally configured, with an isolation valve between the gas chromatograph and mass spectrometer, was unsatisfactory for the identification of hypnotics-sedatives. However, with the capillary inserted directly into the ion source, we could detect 10 ng of these drugs on a total-ion chromatogram. The software programs cause the instrument to be highly automated. In terms of ease of operation and speed it was found suitable for use in a routine clinical laboratory. Chromatography of urine extracts on the capillary gas chromatograph-mass spectrometer yielded excellent resolution of parent compounds and metabolites (e.g., diphenhydramine together with approximately four metabolites and propoxyphene with four metabolites). However, the manufacturer's computer program used to evaluate the quality of the match between the experimental mass spectra and the 375 drug reference spectra was only moderately successful in identifying unknown compounds. The ability of this capillary GC-MS to identify most compounds with a high degree of confidence will be increased by enlarging the library to include more drugs and metabolites and by using a more reliable computerized matching program.


1983 ◽  
Vol 66 (6) ◽  
pp. 1443-1446
Author(s):  
Ray H Liu ◽  
Warren W Ku ◽  
Mary P Fitzgerald

Abstract A gas chromatograph-mass spectrometer-data system equipped with a capillary column is used to analyze commonly abused amine drug mixtures. Enantiomeric amines are analyzed as N-trifluoroacetyl- I-prolyl chloride derivatives. The 10 compounds included in this study are amphetamine, methamphetamine, norephedrine, ephedrine, 3,-4-methylenedioxyamphetamine, N,N-dimethyltryptamine, N,N-diethyltryptamine, N,N-dimethyl-5-methoxytryptamine, mescaline, and caffeine. All compounds, including possible enantiomers, are resolved and identified by the described method.


2018 ◽  
Vol 154 (6) ◽  
pp. S-647
Author(s):  
Constance Bahr ◽  
Peter Moore ◽  
Erin R. Shanahan ◽  
Paul Burn ◽  
Craig Williams ◽  
...  

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