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Analyst

Title:		Determination of acetyl gestagenic steroids in kidney fat by automated supercritical fluid extraction and liquid chromatography ion-trap mass spectrometry
Author(s):		Stolker AA; Zoontjes PW; Schwillens PL; Kootstra PR; van Ginkel LA; Stephany RW; Brinkman UA;
Address:		"National Institute of Public Health and The Environment, Laboratory for Residue Analysis, Bilthoven, The Netherlands. linda.stolker@rivm.nl"
Journal Title:		Analyst
Year:		2002
Volume:		127
Issue:		6
Page Number:		748 - 754
DOI:		10.1039/b201268p
ISSN/ISBN:		0003-2654 (Print) 0003-2654 (Linking)
Abstract:		"Acetyl gestagenic steroids are isolated from animal tissues such as bovine kidney fat by automated supercritical fluid extraction (SFE). After the addition of internal standards and sample pretreatment, the analytes are extracted from the matrix by supercritical CO2 and trapped directly in-line on alumina placed in the extraction vessel. The samples are analysed by liquid chromatography combined with ion-trap mass selective detection (LC-MSn). For quantification, deuterated internal standards are added and single ions of the analytes and internal standards are monitored. For confirmation of the identity of the analytes, two transition ions (one MS2 and one MS3) were monitored and the ratios between the ions were calculated and compared with those of standards. The detection capability for the multi-analyte LC-MSn analysis of megestrol acetate (MA), medroxyprogesterone acetate (MPA), chlormadinone acetate (CMA) and melengestrol acetate (MGA) is 0.5 microg kg(-1). The mean within-laboratory reproducibility ranges from 16-19% (%RSD) at a concentration level of 0.5 microg kg(-1) (n = 9). Running the SFE procedure overnight allows the analysis of 24 samples of fat per day"
Keywords:		Animals Cattle Drug Residues/*analysis Drug and Narcotic Control Growth Substances/*analysis Kidney/*chemistry Melengestrol Acetate/*analysis Veterinary Drugs/*analysis;
Notes:		"MedlineStolker, Alida A M Zoontjes, Paulus W Schwillens, Paulus L W J Kootstra, Peter R van Ginkel, Leendert A Stephany, Rainer W Brinkman, Udo A Th eng England 2002/07/31 Analyst. 2002 Jun; 127(6):748-54. doi: 10.1039/b201268p"