RESUMO
A simple, rapid, sensitive and specific gas chromatography-tandem mass spectrometry (GC-MS/MS) method was developed for quantitation of salbutamol in human urine using salbutamol-d3 as the internal standard. The processing of urines samples includes deconjugation with enzymatic hydrolysis, solid phase extraction procedure utilizing XAD2 column and liquid-liquid extraction accompanied by the derivatization by means of MSTFA/IODO-TMS/DTE mixture. The GC column was a HP Ultra-1 (17 m × 0.22 mm × 0.11 µm) used to separate the peak of interest. The data for GC-MS/MS were acquired and processed utilizing GC Labs Solution and Insight GCMS Software. The detection of spectra was performed on TQ 8050. This method included a chromatographic run of 13.67 min and the linearity was found over the concentration range of 250-2000 ng/mL with a regression coefficient (r2) of 0.99. The coefficient of variation for intra and interday assay precision was between 1.85 and 2.85% and the accuracy was between 95.50 and 107.04% for low quality control (QC), medium QC and high QC. The recovery was adequate to reliable detect the analyte at or below the level recommended by the World Anti-Doping Agency i.e., threshold 1000 ng/mL. The limit of detection and limit of quantification were found to be 10 and 100 ng/mL, respectively. The expanded measurement uncertainty (Uexp%) was found to be 8.28%.
Assuntos
Albuterol , Espectrometria de Massas em Tandem , Humanos , Espectrometria de Massas em Tandem/métodos , Cromatografia Gasosa-Espectrometria de Massas , Incerteza , Cromatografia Líquida/métodosRESUMO
Tamoxifen and toremifene are two selective estrogen receptor modulators (SERMs) commonly used to treat breast cancer in women. Toremifene is well-known as a triphenylethylene derivative. Carboxy toremifene is a common metabolite of toremifene and tamoxifen. Since 2005, the World Anti-Doping Agency (WADA) has banned the SERMs category during in and out of competition. These substances are in the S4 category in the WADA prohibited list as "agents with anti-oestrogenic activity." However, there is no commercially accessible carboxy toremifene reference material in the market. This research highlights the novel synthetic procedure, the development of a carboxy toremifene HPLC method, and validation, along with detailed characterization using advanced analytical techniques using 1 H NMR, HRMS, FT-IR-ATR and UV-visible spectroscopy. RP-HPLC-DAD method was developed and validated to assess the purity of carboxy toremifene. Developed reference material has shown 100% purity. Therefore, we recommend that this synthesized carboxy toremifene may be used as reference material to strengthen the WADA-accredited lab to maintain a clean sports mission during sports competitions.