Detection of thyroid hormones in urine by liquid chromatography coupled to tandem mass spectrometry.

Drug Test Anal

Laboratorio Antidoping FMSI, Federazione Medico Sportiva Italiana, Rome, Italy.

Published: July 2024

AI Article Synopsis

  • A recent study investigated the use of thyroid hormones (TH) in sports for metabolism enhancement, appealing to athletes interested in weight management and increased energy expenditure.
  • The researchers developed and validated a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to measure TH levels in urine, specifically after administration of a diiodothyronine (3,5-T2) supplement.
  • The results showed that 3,5-T2 levels in urine peaked shortly after consumption but returned to baseline within 30 hours, demonstrating the method's effectiveness in detecting TH and its metabolic impact.

Article Abstract

Recently, the trend of thyroid hormones (TH) consumption in the sports community has been published. It is known the capacity of the exogenously administered TH to enhance metabolism, being an attractive feature for athletes, who search for weight control and increased caloric expenditure. This paper aimed the validation of a method to measure TH and related compounds in urine by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method was applied to urine samples collected before and after the administration of a diiodothyronine (3,5-T2) supplement. A method to detect nine TH included an enzymatic hydrolysis, liquid-liquid extraction, and solid-phase extraction. The extracts were analyzed by LC-MS/MS. Validated parameters showed good results for accuracy (85%-104%), precision (3%-16%), LOD (10-40 pg/mL, except for thyronacetic acids that was 200 pg/mL), and the combined uncertainty (2.2%-22%). Maximum concentration of 3,5-T2 in pre-administration samples was 0.71 ng/mL, and after 30 h of the last administration, concentrations returned to pre-administration values. Maximum values of ratios between the analyte and thyronine, T3, and T4 were 0.09, 0.19, and 0.12, respectively, and after 30 h of the last administration, the ratios reached back the basal values. Acidic or basic metabolites were not found in urine at least at the method LOD. A proposed method to assess TH in urine was validated, and as a proof of concept, its efficacy was demonstrated with an excretion study of 3,5-diiodothyronine. The consumption of 3,5-T2 was detected in urine measuring the analyte concentration and ratios between the analyte and thyronine, T3, and T4.

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http://dx.doi.org/10.1002/dta.3764DOI Listing

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