Simultaneous GC-FT-IR/GC-MS Analysis for Isomer-Specific Identification and Quantitation of Complex Mixture Components

1992 ◽  
Vol 46 (2) ◽  
pp. 277-282 ◽  
Author(s):  
N. R. Smyrl ◽  
D. M. Hembree ◽  
W. E. Davis ◽  
D. M. Williams ◽  
J. C. Vance

The construction and capabilities of a new instrument combining infrared and mass spectrometry to simultaneously examine the effluent from a single capillary column gas chromatographic injection are described. Gas chromatography-mass spectrometry (GC-MS) is performed in the conventional manner. However, the Fourier transform infrared (FT-IR) portion of the instrument employs a new sampling method involving low-temperature trapping of the effluent from the gas chromatograph. The mass spectrometer was over two orders of magnitude more sensitive (161 fg detection limit for naphthalene) than the infrared (40 pg). The qualitative capabilities of infrared spectrometry, particularly when isomerspecific identifications are necessary, are shown to be highly complementary to the usual GC-MS method for analyzing complex mixtures

1987 ◽  
Vol 70 (5) ◽  
pp. 912-915 ◽  
Author(s):  
Randall L Smith ◽  
Darryl M Sullivan ◽  
Earl F Richter

Abstract A positive bias in the gas chromatographic (GC) analysis of butter for β-sitosterol was discovered when attempting to confirm values by gas chromatography/mass spectrometry (GC/MS). The source of the problem was traced to an interfering material that was not effectively separated by packed column GC. Because capillary columns are known to provide superior separation, they were substituted for packed columns in the assay, and instrument parameters were modified accordingly. A compound with a similar retention time, identified by GC/MS as lanosterol, was separated from β-sitosterol by the capillary column. The capillary column technique was applied to over 300 butter samples. The results indicate that the method can accurately quantitate β-sitosterol in butter with no known interferences. The limit of detection for this method is 1 mg/100 g. Recoveries at a level of 3 mg/100 g averaged 98% with a coefficient of variation of 3.45%


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.


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