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Anal Bioanal Chem ; 405(1): 331-40, 2013 Jan.
Article in English | MEDLINE | ID: mdl-23064711

ABSTRACT

We have developed a simple and sensitive method for the simultaneous determination of testosterone (TES), cortisol (CRT), and dehydroepiandrosterone (DHEA) in saliva by automated online in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) using a Discovery HS F5 column. The optimum in-tube SPME conditions were 25 draw/eject cycles of 40 µL of sample at a flow rate of 200 µL/min using a Supel-Q PLOT capillary column as an extraction device. The extracted compounds were easily desorbed from the capillary by passage of the mobile phase, and no carryover was observed. The in-tube SPME LC-MS/MS method showed good linearity with correlation coefficients r ≥ 0.9998 for TES, CRT, and DHEA using their respective stable isotope-labeled internal standards. The intra-day and inter-day precisions (relative standard deviations) were below 4.9 and 8.5 % (n = 5), respectively. This method was successfully utilized to analyze TES, CRT, and DHEA in saliva samples without any other pretreatment or interference peaks, and the quantification limits (S/N = 10) of TES, CRT and DHEA were about 0.01, 0.03 and 0.29 ng/mL saliva, respectively. The recoveries of these compounds spiked into saliva samples were each above 94%. This method was applied to analyze changes in salivary TES, CRT, and DHEA levels resulting from stress and fatigue load.


Subject(s)
Chromatography, Liquid/methods , Dehydroepiandrosterone/analysis , Hydrocortisone/analysis , Saliva/metabolism , Solid Phase Microextraction/methods , Tandem Mass Spectrometry/methods , Testosterone/analysis , Chemistry Techniques, Analytical , Humans , Isotopes/analysis , Models, Chemical , Reproducibility of Results , Stress, Mechanical , Time Factors
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