Irina Zolkina (Presenter)
Pirogov Russian National Research Medical University
Bio: i am doing developments in area quantitative determination of drugs and some biomarkers like a amino acids/purines pyrimidines/organic acids, hormones and other in biofluids (plasma, serum, urine, saliva)
Authorship: S.V. Kovalev, I.V. Zolkina, N.V. Lifantseva, I.S. Mamedov, P.B. Glagovsky
Pirogov Russian National Research Medical University (RNRMU)
| Short Abstract Purpose. Development and validation of methods for determining plasma concentrations of etonogestrel (3-keto desogestrel). The method used - HPLC/MS. Analytical equipment - liquid chromatograph and a mass spectrometer with a triple quadrupole. Chromatographic conditions: analytical column C18 (75*2,1 mm, 3.5 µm), flow rate 0.4 ml/min, eluting with a gradient system (acetonitrile :water). Detection mode is MRM. Sample preparation is a liquid-liquid extraction with diethyl ether was concentrated and redissolved in 50% acetonitrile. Results. The recovery rate is 77%. Calibration curve is linear in the range 40-4000 pg/ml. The LLOQ is 40 pg/ml and LOD is 20 pg/ml. Conclusions. Etonogestrel - active substance in the composition of many last-generation oral contraceptives. The method developed by HPLC/MS is sensitive enough to determine the picogram of etonogestrel in human plasma. |
Long Abstract
Purpose. Development and validation of methods for determining plasma concentrations picogram etonogestrel (3-keto desogestrel) - active metabolite of desogestrel (oral contraceptive last generation), as well as its application to studies of bioequivalence and pharmacokinetics.
Materials and methods. The method used - HPLC / MS. Analytical equipment - liquid chromatograph Shimadzu (Japan) and a mass spectrometer with a triple quadrupole ABSciex QTrap 4500 (USA). Chromatographic conditions: precolumn Agilent Zorbax XDB-C8 (12,5*2,1 mm grain size 5 microns), column Agilent Zorbax Eclipse XDB-C18 (75*2,1 mm grain size 3.5 microns), flow rate 0.4 ml/min, eluting with a gradient system of acetonitrile and water from 50 to 100% acetonitrile. For the selective detection mode is MRM (Multiple Reaction Monitoring). Sample preparation is a liquid-liquid extraction with diethyl ether was concentrated and redissolved in 50% acetonitrile.
Results. The recovery rate is 77%. Calibration curve is linear in the defined range of values (40-4000 pg/ml). The lower limit of quantification of 40 pg/ml. The detection limit of 20 pg/ml. The technique developed by the standards of FDA and EMEA, as well as used for the analysis of plasma samples of volunteers in the study, bioequivalence of the two formulations of desogestrel.
Conclusions. Etonogestrel - active substance in the composition of many last-generation oral contraceptives. Methods of analysis it is necessary to research on the pharmacokinetics and bioequivalence of drugs containing it. The method developed by HPLC/MS is sensitive enough to determine the picogram of etonogestrel in human plasma.
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