Ultra-performance liquid chromatography-tandem mass spectrometry assay for determination of plasma nomegestrol acetate and estradiol in healthy postmenopausal women
| Autor: | Sneha G. Nair, Puran Singhal, Mallika Sanyal, Daxesh P. Patel, Pranav S. Shrivastav |
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| Rok vydání: | 2017 |
| Předmět: |
Nomegestrol acetate
Adult Norpregnadienes Clinical Biochemistry Mass spectrometry 01 natural sciences Biochemistry High-performance liquid chromatography Sensitivity and Specificity Analytical Chemistry 03 medical and health sciences chemistry.chemical_compound 0302 clinical medicine Liquid chromatography–mass spectrometry Tandem Mass Spectrometry Drug Discovery Humans Solid phase extraction Derivatization Molecular Biology Chromatography High Pressure Liquid Aged Pharmacology Dansyl Compounds 030219 obstetrics & reproductive medicine Chromatography Estradiol 010401 analytical chemistry Dansyl chloride Extraction (chemistry) Reproducibility of Results General Medicine Megestrol Middle Aged 0104 chemical sciences Postmenopause chemistry Linear Models Female |
| Zdroj: | Biomedical chromatography : BMC. 32(2) |
| ISSN: | 1099-0801 |
| Popis: | A highly sensitive and selective ultra-performance liquid chromatography-tandem mass spectrometry method is described for the simultaneous determination of nomegestrol acetate (NOMAC), a highly selective progestogen, and estradiol (E2), a natural estrogen in human plasma. NOMAC was obtained from plasma by solid phase extraction, while E2 was first separated by liquid-liquid extraction with methyl tert-butyl ether followed by derivatization with dansyl chloride. Deuterated internal standards, NOMAC-d5 and E2-d4 were used for better control of extraction conditions and ionization efficiency. The assay recovery of the analytes was within 90-99 %. The analytes were separated on UPLC BEH C18 (50 × 2.1 mm, 1.7 μm) column using a mobile phase comprising of acetonitrile and 3.0 mM ammonium trifluoroacetate in water (80:20, v/v) with a resolution factor (Rs) of 3.21. The calibration curves were linear from 0.01-10.0 ng/mL for NOMAC and 1.00-1000 pg/mL for E2, respectively. The intra-batch and inter-batch precision was ≤5.8 % and the accuracy of quality control samples ranged from 96.7 to 103.4 % for both the analytes. The practical applicability of the method is demonstrated by analyzing samples from 18 healthy postmenopausal women after oral administration of 2.5 mg nomegestrol acetate and 1.5 mg estradiol film coated tablets under fasting. |
| Databáze: | OpenAIRE |
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