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Determination of raloxifene and its glucuronides in human urine by liquid chromatography-tandem mass spectrometry assay
Trdan Lušin, Tina (Author), Roškar, Robert (Author), Trontelj, Jurij (Author), Ravnikar, Matjaž (Author), Mrhar, Aleš (Author)

URLURL - Presentation file, Visit http://www.sciencedirect.com/science/article/pii/S1570023211004168 This link opens in a new window

Abstract
A selective, sensitive, accurate and precise liquid chromatography-tandem massspectrometry (LC-MS/MS) method for determination of raloxifene and its three glucuronides: raloxifene6 bglucuronide (M1), raloxifene4 0 bglucuronide (M2), raloxifene6,4 0diglucuronide (M3) in urine samples is presented in this paper. To our knowledge the developed analytical method is the first fully validated method capable of simultaneous determination of raloxifene and its glucuronides in real urine samples. Moreover, for the first time a method for determination of raloxifene diglucuronide in relevant biological samples was introduced. Metabolites were obtained by a bioconversion process of raloxifeneto its glucuronides using the microorganism Streptomyces sp. and were used as standards for validation. Urine samples were introduced to a simple solid phase extraction prior to the analysis by LC-MS/MS. The method was linear in a wide range with high determination coefficient (r2 > 0.997). The limits of quantification achieved were 1.01, 1.95, 2.83 and 4.69 nM for raloxifene, M1, M2 and M3, respectively. The recoveries were higher than 92.5%, the accuracy was within 100 8.8% and the precision was better than 12% for all compounds. The developed method was successfully applied to the real urine samples and showed to be appropriate for use in further research ofstill not completely discovered raloxifene pharmacokinetics. Furthermore, the presented method could also serve for a potential application in antidoping analysis.

Language:English
Keywords:raloksifen, urin, farmakokinetika, doping
Work type:Not categorized (r6)
Tipology:1.01 - Original Scientific Article
Organization:FFA - Faculty of Pharmacy
Year:2011
Number of pages:str. 2323-2331
Numbering:Vol. 879, issue 23
UDC:542+615.015
ISSN on article:1570-0232
DOI:10.1016/j.jchromb.2011.06.031 Link is opened in a new window
COBISS.SI-ID:3063409 Link is opened in a new window
Views:726
Downloads:192
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Record is a part of a journal

Title:Journal of chromatography
Publisher:Elsevier
ISSN:1570-0232
COBISS.SI-ID:2817144 This link opens in a new window

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