TY - JOUR T1 - Automated solid-phase extraction for concentration and clean-up of female steroid hormones prior to liquid chromatography-electrospray ionization-tandem mass spectrometry: an approach to lipidomics. AU - Alvarez Sánchez,B, AU - Capote,F Priego, AU - Jiménez,J Ruiz, AU - Luque de Castro,M D, Y1 - 2008/08/29/ PY - 2008/03/27/received PY - 2008/08/10/revised PY - 2008/08/14/accepted PY - 2008/9/16/pubmed PY - 2008/12/17/medline PY - 2008/9/16/entrez SP - 46 EP - 54 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1207 IS - 1-2 N2 - A method for determination of free and glucuronide-conjugated female steroid hormones in urine at the pgmL(-1) level is here presented. For this purpose, a dual approach with or without beta-glucuronidase hydrolysis has been developed to succeed in this analysis. The target analytes were two progestogens - progesterone and pregnenolone - and three endogenous estrogens - estradiol, estriol and estrone. Separation and detection were carried out by liquid chromatography electrospray ionization and tandem mass spectrometry (LC-ESI-MS-MS) with a triple quadrupole (qQq) mass detector. The determination step was optimized by multiple reaction monitoring for highly selective identification and sensitive quantification of female hormones in a complex sample such as human urine. As these compounds are present in urine at very low concentration (ngmL(-1) level), a preconcentration and clean-up step by solid-phase extraction was automatically carried out prior to the chromatographic step in order to improve the sensitivity of the method. This sample pretreatment was performed using a lab-on-valve (LOV) manifold which provided preconcentration factors ranging from 59.1 to 72.3 for 10mL urine. The detection and quantification limits were in the ranges 1.8-18pg and 6-61pg on-column, respectively, with precision values from 1.93 to 10.99%, expressed as relative standard deviation. These results enable to conclude the suitability of the LOV-LC-qQq approach for determination of the lipidomic profiling of the main female steroid hormones in a difficult matrix as human urine. The method can be potentially applied to the clinical and other metabolomic areas. SN - 0021-9673 UR - https://www.unboundmedicine.com/medline/citation/18790493/Automated_solid_phase_extraction_for_concentration_and_clean_up_of_female_steroid_hormones_prior_to_liquid_chromatography_electrospray_ionization_tandem_mass_spectrometry:_an_approach_to_lipidomics_ DB - PRIME DP - Unbound Medicine ER -