Determination of sterol and triterpene alcohol acetates in natural products by reversed-phase liquid chromatography and gas chromatography—mass spectrometry

1985 ◽  
Vol 329 ◽  
pp. 231-246 ◽  
Author(s):  
Jean-Pierre Bianchini ◽  
Emile M. Gaydou ◽  
Jean-Claude Sigoillot ◽  
Gérard Terrom
2004 ◽  
Vol 87 (1) ◽  
pp. 107-115 ◽  
Author(s):  
Francesca Calbiani ◽  
Maria Careri ◽  
Lisa Elviri ◽  
Alessandro Mangia ◽  
Ingrid Zagnon

Abstract A rapid and accurate method using reversed-phase liquid chromatography–tandem mass spectrometry interfaced with electrospray was developed for determination of acrylamide in cooked food samples. A simplified sample treatment procedure using an extraction step with acidified water without cleanup was developed. A C18 column with an aqueous formic acid–methanol mixture as the mobile phase was used under isocratic conditions. The method was validated in-house for robustness, limits of detection (LOD) and quantitation (LOQ), linearity, recovery, and accuracy both on standard and baked-product and potato flour matrixes. Good results in the low ppb level were obtained for LOD (<15 μg/kg) and LOQ (<25 μg/kg) of acrylamide in samples. Excellent linearity (r 2 = 0.999–1.000) was established over 2 orders of magnitude by performing statistical tests. The absence of both constant and proportional systematic errors demonstrated good method accuracy. Excellent results were obtained for intraday repeatability (RSD < 1.5%) and between-day precision (RSD < 5%). Extraction recoveries from food products were calculated in the 97 ± 3–99 ± 2% (n = 6) range with a labeled internal standard (13C3-acrylamide). The applicability of the method to determination of acrylamide in cooked food products was demonstrated.


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.


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