Investigation of on-line reversed-phase liquid chromatography–gas chromatography–mass spectrometry as a tool for the identification of impurities in drug substances

The Analyst ◽  
1996 ◽  
Vol 121 (1) ◽  
pp. 61-66 ◽  
Author(s):  
Elise C. Goosens ◽  
Karel H. Stegman ◽  
Dirk de Jong ◽  
Gerhardus J. de Jong ◽  
Udo A. Th Brinkman
1979 ◽  
Vol 51 (14) ◽  
pp. 2324-2328 ◽  
Author(s):  
B. L. Karger ◽  
D. P. Kirby ◽  
Paul. Vouros ◽  
R. L. Foltz ◽  
B. Hidy

Author(s):  
N Ashraf-Khorassani ◽  
N Nazem ◽  
LT Taylor ◽  
WM Coleman

AbstractGas chromatography-mass spectrometry (GC-MS) and reversed-phase liquid chromatography-mass spectrometry (LC-MS) were used to compare and quantify sucrose esters (SE) in five different tobaccos. The concentration of SE varied from 340 to 950 µg/g. In order to quantify the SE in each tobacco, the trimethylsilane (TMS) derivative of each sample was analyzed via GC-MS. It appeared that in the five tobaccos, the intensities of the five chosen SE-derived molecular masses increased in the order m/z 622 < 636 < 678 < 650 < 664 for samples 1-3, but for samples 4 and 5, the m/z 678 and 650 were reversed. In order to qualitatively characterize the various SE chromatographic fractions LC-MS was used. It was determined that the lowest parent SE m/z in which acetyl was attached to glucose was detected at m/z 566 (10 carbons), and the highest m/z was found at 692 (19 carbons). Some m/z values showed more than one peak which indicated the presence of isomers. All samples showed the presence of at least five different SE peaks wherein acetyl was attached to fructose (i.e. m/z 205). Also, acyl unsaturation was observed in selected fractions.


2011 ◽  
Vol 74 (6) ◽  
pp. 960-966 ◽  
Author(s):  
R. M. MARTÍNEZ ◽  
C. BARBA ◽  
M. M. CALVO ◽  
G. SANTA-MARÍA ◽  
M. HERRAIZ

The use of on-line coupling of reversed-phase liquid chromatography and gas chromatography (RPLC-GC) with the through oven transfer adsorption desorption (TOTAD) interface and mass spectrometry (MS) was proposed for testing different types of commercial Spanish dry-cured ham for irradiation treatment at various doses (0, 1.5, 2, and 4 kGy). The qualitative analysis of radiation-specific compounds (e.g., n-pentadecane, 1-hexadecene, 1,7-hexadecadiene, n-heptadecane, 8-heptadecene, and 2-dodecylcyclobutanone) can be simultaneously established in a single run with samples that have or have not been irradiated. The overall analysis, which takes less than 100 min, includes a rapid extraction step using a small amount of dichloromethanemethanol (1:1, vol/vol) and anhydrous sodium sulfate, the subsequent fractionation of the sample in the first dimension of the system (RPLC), the transfer of the target fraction to the second dimension, the GC separation, and the MS detection. The calculated limits of detection in ham were lower than 22 ng/g. Repeatability studies provided relative standard deviation values of 0.8 to 13.5%.


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