A robust LC–MS/MS assay with online cleanup for measurement of serum testosterone

Autor: Sihe Wang, Yu Zhou
Rok vydání: 2019
Předmět:
Zdroj: Journal of Separation Science. 42:2561-2568
ISSN: 1615-9314
1615-9306
DOI: 10.1002/jssc.201801189
Popis: Accurate measurement of low levels of testosterone is critical for diagnosis and treatment of androgen disorders. The very low concentrations of testosterone in children, females, and males with androgen suppression therapies necessitate the use of mass spectrometry-based methods. We aimed to develop a liquid chromatography with tandem mass spectrometry method with simplified sample preparation and online solid-phase extraction cleanup to achieve enhanced precision, accuracy, robustness, and cost-effectiveness. The assay was linear from 10 to 20 000 pg/mL with an analytical recovery of 93-104%. The total coefficient of variation was 2.5, 1.9, and 1.7% at concentration levels of 348, 5432, and 10 848 pg/mL, respectively. No significant carryover was observed from samples with concentrations up to 20 000 pg/mL. No significant interference was observed from androstenedione, dehydroepiandrosterone, epi-testosterone, and estriol. Comparison with CDC Hormone Standardization program (HoSt) reference samples with defined values (n = 40) showed a Deming regression slope of 0.963, intercept of 28.06 pg/mL, standard error of estimate was 66.9, a correlation coefficient of 0.9996, and a mean bias of -0.6%. The method met the accuracy criteria by the CDC HoSt program. In addition, we achieved >12 000 injections on a single analytical column without significant performance deterioration due to the specific online solid-phase extraction settings.
Databáze: OpenAIRE
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