title: Rapid and sensitive method for quantification of gestodene in human plasma as the oxime derivative by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and its application to bioequivalence study.
abstract: A rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the estimation of gestodene in human plasma. Gestodene was extracted from human plasma by using solid-phase extraction technique. Gestodene D6 was used as the internal standard. An Acquity HSS-T3 column provided chromatographic separation of analytes followed by detection with mass spectrometry. The mass transition ion-pair was followed as m/z 326.2→124.1 for gestodene and m/z 332.3→129.1 for gestodene D6. The method involves a solid phase extraction from plasma, rapid derivatization with hydroxylamine to form oxime, simple gradient chromatographic conditions and mass spectrometric detection that enables detection at sub-picogram levels. The proposed method has been validated for a linear range of 50-11957pg/ml with a correlation coefficient≥0.9994. The intra-run and inter-run precision and accuracy were within 10%. The overall recoveries for gestodene and gestodene D6 were 62.02% and 67.57% respectively. The total run time was 4.0min. The developed method was applied for the determination of the pharmacokinetic parameters of gestodene following a single oral administration of a 2×0.06mg gestodene tablets in 10 healthy female volunteers.
authors.affiliation: Bioanalytical Research Department, Lupin Bio-Research Center, Pashan, Pune 411021, Maharastra, India; Department of Pharmacy, Pacific University, P.B.-12 Pacific Hills, Airport Road, Pratap Nagar Extension, Debari, Udaipur 313024, Rajasthan, India. Electronic address: ashishsaxena@lupinpharma.com.
authors.forename: Ashish
authors.initials: A
authors.lastname: Saxena
authors.affiliation: Department of Pharmacy, Pacific University, P.B.-12 Pacific Hills, Airport Road, Pratap Nagar Extension, Debari, Udaipur 313024, Rajasthan, India.
authors.forename: Arun
authors.initials: A
authors.lastname: Gupta
authors.affiliation: Bioanalytical Research Department, Lupin Bio-Research Center, Pashan, Pune 411021, Maharastra, India.
authors.forename: Ravisekhar
authors.initials: R
authors.lastname: Kasibhatta
authors.affiliation: Bioanalytical Research Department, Lupin Bio-Research Center, Pashan, Pune 411021, Maharastra, India.
authors.forename: Manoj
authors.initials: M
authors.lastname: Bob
authors.affiliation: Bioanalytical Research Department, Lupin Bio-Research Center, Pashan, Pune 411021, Maharastra, India.
authors.forename: V Praveen
authors.initials: VP
authors.lastname: Kumar
authors.affiliation: Bioanalytical Research Department, Lupin Bio-Research Center, Pashan, Pune 411021, Maharastra, India.
authors.forename: Bipin
authors.initials: B
authors.lastname: Purwar
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods; D003280:Contraceptives, Oral, Synthetic / Q000097:blood*; D005260:Female; D006801:Humans; D057230:Limit of Detection; D009652:Norpregnenes / Q000097:blood*; D010091:Oximes / Q000097:blood*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013810:Therapeutic Equivalency
chemical_list: D003280:Contraceptives, Oral, Synthetic; D009652:Norpregnenes; D010091:Oximes; C033273:Gestodene
keywords: Gestodene; Human plasma; Hydroxylamine; LC–MS/MS; Oxime derivative