Ultra-performance liquid chromatography-tandem mass spectrometry assay for determination of plasma nomegestrol acetate and estradiol in healthy postmenopausal women.
Biomed Chromatogr
; 32(2)2018 Feb.
Article
in En
| MEDLINE
| ID: mdl-28869284
ABSTRACT
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 (8020, v/v) with a resolution factor (Rs ) of 3.21. The calibration curves were linear from 0.01 to 10.0 ng/mL for NOMAC and from 1.00 to 1000 pg/mL for E2, respectively. The intra- and inter-batch precision was ≤5.8% and the accuracy of quality control samples ranged from 96.7 to 103.4% for both 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.
Key words
Full text:
1
Collection:
01-internacional
Database:
MEDLINE
Main subject:
Chromatography, High Pressure Liquid
/
Postmenopause
/
Estradiol
/
Tandem Mass Spectrometry
/
Megestrol
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Norpregnadienes
Type of study:
Diagnostic_studies
/
Guideline
/
Prognostic_studies
Limits:
Adult
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Aged
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Female
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Humans
/
Middle aged
Language:
En
Journal:
Biomed Chromatogr
Year:
2018
Type:
Article
Affiliation country:
India