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Analysis of corticosteroids in urine by HPLC and thermospray LC/MS.
J Anal Toxicol. 1990 Mar-Apr; 14(2):102-8.JA

Abstract

The method for simultaneous determination and confirmation of nine corticosteroids in urine by high-performance liquid chromatography with a diode array detector and thermospray liquid chromatography-mass spectrometry was studied. HPLC was performed on a C18 column with a gradient mobile phase system of water and acetonitrile. The calibration curve was linear from 20 ng/mL to 1.0 micrograms/mL for each corticosteroid, and the detection limit was 10 ng/mL in 5 mL of urine. The extraction recovery of each corticosteroid from the spiked urine was equal to or greater than 85% by liquid-liquid extraction (LLE) at pH 9 using diethyl ether and approximately 79% or more by solid-phase extraction (SPE) with a Sep-Pak C18 cartridge. The mass spectra obtained with the positive ion mode showed protonated molecular species [M + H]+, ammonium adduct ion [M + NH4]+, [MH-60]+, [MH-30]+, and [MH-18]+. The LC/MS detection limits ranged from 10 to 50 ng in the scan mode and from 1 to 5 ng in the selected ion monitoring (SIM) mode.

Authors+Show Affiliations

Doping Control Center, Korea Institute of Science and Technology, Cheongryang, Seoul.No affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

1691351

Citation

Park, S J., et al. "Analysis of Corticosteroids in Urine By HPLC and Thermospray LC/MS." Journal of Analytical Toxicology, vol. 14, no. 2, 1990, pp. 102-8.
Park SJ, Kim YJ, Pyo HS, et al. Analysis of corticosteroids in urine by HPLC and thermospray LC/MS. J Anal Toxicol. 1990;14(2):102-8.
Park, S. J., Kim, Y. J., Pyo, H. S., & Park, J. (1990). Analysis of corticosteroids in urine by HPLC and thermospray LC/MS. Journal of Analytical Toxicology, 14(2), 102-8.
Park SJ, et al. Analysis of Corticosteroids in Urine By HPLC and Thermospray LC/MS. J Anal Toxicol. 1990 Mar-Apr;14(2):102-8. PubMed PMID: 1691351.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Analysis of corticosteroids in urine by HPLC and thermospray LC/MS. AU - Park,S J, AU - Kim,Y J, AU - Pyo,H S, AU - Park,J, PY - 1990/3/1/pubmed PY - 1990/3/1/medline PY - 1990/3/1/entrez SP - 102 EP - 8 JF - Journal of analytical toxicology JO - J Anal Toxicol VL - 14 IS - 2 N2 - The method for simultaneous determination and confirmation of nine corticosteroids in urine by high-performance liquid chromatography with a diode array detector and thermospray liquid chromatography-mass spectrometry was studied. HPLC was performed on a C18 column with a gradient mobile phase system of water and acetonitrile. The calibration curve was linear from 20 ng/mL to 1.0 micrograms/mL for each corticosteroid, and the detection limit was 10 ng/mL in 5 mL of urine. The extraction recovery of each corticosteroid from the spiked urine was equal to or greater than 85% by liquid-liquid extraction (LLE) at pH 9 using diethyl ether and approximately 79% or more by solid-phase extraction (SPE) with a Sep-Pak C18 cartridge. The mass spectra obtained with the positive ion mode showed protonated molecular species [M + H]+, ammonium adduct ion [M + NH4]+, [MH-60]+, [MH-30]+, and [MH-18]+. The LC/MS detection limits ranged from 10 to 50 ng in the scan mode and from 1 to 5 ng in the selected ion monitoring (SIM) mode. SN - 0146-4760 UR - https://www.unboundmedicine.com/medline/citation/1691351/Analysis_of_corticosteroids_in_urine_by_HPLC_and_thermospray_LC/MS_ L2 - https://academic.oup.com/jat/article-lookup/doi/10.1093/jat/14.2.102 DB - PRIME DP - Unbound Medicine ER -