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Rapid determination of corticosteroids in urine by combined solid phase microextraction/liquid chromatography/mass spectrometry
Author(s) -
Volmer Dietrich A.,
Hui Joseph P. M.
Publication year - 1997
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/(sici)1097-0231(199711)11:17<1926::aid-rcm97>3.0.co;2-2
Subject(s) - chemistry , chromatography , solid phase microextraction , mass spectrometry , detection limit , urine , extraction (chemistry) , sample preparation , analytical chemistry (journal) , gas chromatography–mass spectrometry , biochemistry
Solid‐phase microextraction combined with first short‐column liquid chromatography/mass spectrometry (SPME/LC/MS) was used for isolating and analysing 11 corticosteroids and 2 steroid conjugates from urine samples. Several SPME parameters such as polarity of fibres, extraction time and effect of ionic strengh, were investigated, and their impact on the SPME/LC/MS technique was studied. To demonstrate the potential of the SPME/LC/MS method, its application to the determination of steroids in human urine was investigated. The method was shown to be sensitive with detection limits between 4 and 300 ng/mL and precision between 4.9 and 11.1% RSD through the use of an internal standard technique. The versatility of the method was also exhibited by its excellent linearity in the concentration range of 20 to 20 000 ng/mL in urine for all investigated compounds. A comparison of the SPME/LC/MS method with LC/MS methods utilizing traditional sample preparation techniques, shows that the former offers similar performance in terms of precision, linearity and detection limits, but is clearly easier to use and faster to perform. © 1997 John Wiley & Sons, Ltd.