SPE-UPLC-MS/MS assay for determination of letrozole in human plasma and its application to bioequivalence study in healthy postmenopausal Indian women
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摘要
A rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method is described for determination of letrozole in human plasma.Following solid phase extraction(SPE) of letrozole and letrozole-d4 on Orochem DVB-LP cartridges,chromatography was performed on Acquity UPLC BEH C_(18)(50 mm × 2.1 mm.1.7 μm) column using methanol-0.1%formic acid in water(85:15,v/v) as the mobile phase.Detection was carried out on a triple quadrupole mass spectrometer with an electrospray source,operated under positive ionization mode.Quantitation of letrozole and letrozole-d4 was done using multiple reaction monitoring(MRM) following the transitions at m/z286.2→217.0 and m/z 290.2→221.0,respectively.The calibration plots were linear through the concentration range of 0.10-100 ng/mL(r~2 ≥ 0.9990) using 100 μL human plasma.The extraction recovery of letrozole ranged from 94.3%to 96.2%and the intra-batch and inter-batch precision was ≤ 5.2%.The method was successfully applied to a bioequivalence study of letrozole after oral administration of2.5 mg tablet formulation to 16 healthy postmenopausal Indian women.The assay reproducibility was also established through incurred sample reanalysis(ISR) of 74 subject samples.
A rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method is described for determination of letrozole in human plasma.Following solid phase extraction(SPE) of letrozole and letrozole-d4 on Orochem DVB-LP cartridges,chromatography was performed on Acquity UPLC BEH C_(18)(50 mm × 2.1 mm.1.7 μm) column using methanol-0.1%formic acid in water(85:15,v/v) as the mobile phase.Detection was carried out on a triple quadrupole mass spectrometer with an electrospray source,operated under positive ionization mode.Quantitation of letrozole and letrozole-d4 was done using multiple reaction monitoring(MRM) following the transitions at m/z286.2→217.0 and m/z 290.2→221.0,respectively.The calibration plots were linear through the concentration range of 0.10-100 ng/mL(r~2 ≥ 0.9990) using 100 μL human plasma.The extraction recovery of letrozole ranged from 94.3%to 96.2%and the intra-batch and inter-batch precision was ≤ 5.2%.The method was successfully applied to a bioequivalence study of letrozole after oral administration of2.5 mg tablet formulation to 16 healthy postmenopausal Indian women.The assay reproducibility was also established through incurred sample reanalysis(ISR) of 74 subject samples.
A rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method is described for determination of letrozole in human plasma.Following solid phase extraction(SPE) of letrozole and letrozole-d4 on Orochem DVB-LP cartridges,chromatography was performed on Acquity UPLC BEH C_(18)(50 mm × 2.1 mm.1.7 μm) column using methanol-0.1%formic acid in water(85:15,v/v) as the mobile phase.Detection was carried out on a triple quadrupole mass spectrometer with an electrospray source,operated under positive ionization mode.Quantitation of letrozole and letrozole-d4 was done using multiple reaction monitoring(MRM) following the transitions at m/z286.2→217.0 and m/z 290.2→221.0,respectively.The calibration plots were linear through the concentration range of 0.10-100 ng/mL(r~2 ≥ 0.9990) using 100 μL human plasma.The extraction recovery of letrozole ranged from 94.3%to 96.2%and the intra-batch and inter-batch precision was ≤ 5.2%.The method was successfully applied to a bioequivalence study of letrozole after oral administration of2.5 mg tablet formulation to 16 healthy postmenopausal Indian women.The assay reproducibility was also established through incurred sample reanalysis(ISR) of 74 subject samples.
引文
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[10]R.Shao,LY.Yu,H.G.Lou,et al.,Development and validation of a rapid LC-MS/MS method to quantify letrozole in human plasma and its application to therapeutic drug monitoring,Biomed.Chromatogr.30(2016)632-637.
[11]G.Cao,Q,Zhang,X.Yang,Determination of letrozole in rat plasma by UPLCMS/MS and its application to a pharmacokinetic study,LaL Am.J.Pharm.34(2015)45-50.
[12]S.K.Acharjya,S.K.Bhattamisra,B.R.E.Muddana,et al.,Development of a highperformance liquid chromatographic method for determination of letrozole in wistar rat serum and its application in pharmacokinetic studies,Sci.Pharm.80(2012)941-953.
[13]J.C.Precht,B.Ganchev,G.Heinkele,et al.,Simultaneous quantitative analysis of letrozole,its carbinol metabolite,and carbinol glucuronide in human plasma by LC-MS/MS,Anal.Bioanal.Chem.403(2012)301-308.
[14]J.Rodriguez,G.Castaneda,L Munoz,Rapid determination of letrozole,citalopram and their metabolites by high performance liquid chromatographyfluorescence detection in urine:Method validation and application to real samples,J.Chromatogr.B 913-914(2013)12-18.
[15]B.Beer,B.Schubert,A.Oberguggenberger,et al.,Development and validation of a liquid chromatography-tandem mass spectrometry method for the simultaneous quantification of tamoxifen,anastrozole,and letrozole in human plasma and its application to a clinical study.Anal.Bioanal.Chem.398(2010)1791-1800.
[16]Guidance for Industry,Bionanalytical Method Validation,US Department of Health and Human Services,Food and Drug Administration Centre for Drug Evaluation and Research(CDER),Centre for Veterinary Medicine(CVM),2001.
[17]PA Shah,P.Sharma,J.V.Shah,et al.,An improved LC-MS/MS method for the simultaneous determination of pyrazinamide,pyrazinoic acid and 5-hydroxy pyrazinoic acid inhuman plasma for a pharmacokinetic study,J.Chromatogr.B1017(2016)52-61.
[18]Guidance for Industry:ICH E6 Good Clinical Practice.US.Department of Health and Human Services,Food and Drug Administration,Centre for Drug Evaluation and Research(CDER),Centre for Biologies Evaluation and Research(CBER).1996.
[19]M.Yadav,P.S.Shrivastav,Incurred sample reanalysis(ISR):a decisive tool in bioanalytical research,Bioanalysis 3(2011)1007-1024.
[2]CM.Keating,Letrozole:a review of its use in the treatment of postmenopausal women with hormone-responsive early breast cancer.Drugs 69(2009)1681-1705.
[3]A.Zarghi,S.M.Foroutan,A.Shafaati,et al.,HPLC determination of letrozole in plasma using fluorescence detection:application to pharmacokinetic studies,Chromatographia 66(2007)747-750.
[4]V.Sekar,S.Jayaseelan.N.Subash.et al.,Bioanalytical method development and validation of letrozole by RP-HPLC method,Int J.Pharm.Res.Dev.1(2009)1-7.
[5]M.Rezaee,Y.Yamini,M.Hojjati,et al.,Novel extraction method based on the dispersion of the extraction solvent for extraction of letrozole from biological fluids.Anal.Methods 2(2010)1341-1345.
[6]A.Filipe,S.Almeida,A.C.F.Spinola,et al.,Bioequivalence study of two letrozole tablet formulations.Single dose,randomized,open-label,two-way crossover bioequivalence study of letrozole 2.5 mg tablets in healthy volunteers under fasting conditions,Arzneim.Forsch.58(2008)419-422.
[7]C.Joshi,S.Vishnubhatla,S.Chakkirala,et al.,Validation and application of a high performance liquid chromatography-tandem mass spectrometry assay for letrozole in human plasma,Asian J.Pharm.Clin.Res.4(2011)107-112.
[8]J.Song,Y.Zhan,X.Chen,et al.,Quantification of letrozole in human plasma using LC-(-)ESI-MS/MS with d4-letrozole as internal standard:application in a pharmacokinetic study,J.Liq.Chromatogr.Relat Technol.36(2013)1762-1776.
[9]A.I.Platova,I.I.Miroshnichenko,S.N.Ptitsina,et al.,Rapid and sensitive LC-MS/MS assay for quantitation of Letrozole using solid-phase extraction from human blood plasma and its application to pharmacokinetic studies.Pharm.Chem.J.48(2014)292-297.
[10]R.Shao,LY.Yu,H.G.Lou,et al.,Development and validation of a rapid LC-MS/MS method to quantify letrozole in human plasma and its application to therapeutic drug monitoring,Biomed.Chromatogr.30(2016)632-637.
[11]G.Cao,Q,Zhang,X.Yang,Determination of letrozole in rat plasma by UPLCMS/MS and its application to a pharmacokinetic study,LaL Am.J.Pharm.34(2015)45-50.
[12]S.K.Acharjya,S.K.Bhattamisra,B.R.E.Muddana,et al.,Development of a highperformance liquid chromatographic method for determination of letrozole in wistar rat serum and its application in pharmacokinetic studies,Sci.Pharm.80(2012)941-953.
[13]J.C.Precht,B.Ganchev,G.Heinkele,et al.,Simultaneous quantitative analysis of letrozole,its carbinol metabolite,and carbinol glucuronide in human plasma by LC-MS/MS,Anal.Bioanal.Chem.403(2012)301-308.
[14]J.Rodriguez,G.Castaneda,L Munoz,Rapid determination of letrozole,citalopram and their metabolites by high performance liquid chromatographyfluorescence detection in urine:Method validation and application to real samples,J.Chromatogr.B 913-914(2013)12-18.
[15]B.Beer,B.Schubert,A.Oberguggenberger,et al.,Development and validation of a liquid chromatography-tandem mass spectrometry method for the simultaneous quantification of tamoxifen,anastrozole,and letrozole in human plasma and its application to a clinical study.Anal.Bioanal.Chem.398(2010)1791-1800.
[16]Guidance for Industry,Bionanalytical Method Validation,US Department of Health and Human Services,Food and Drug Administration Centre for Drug Evaluation and Research(CDER),Centre for Veterinary Medicine(CVM),2001.
[17]PA Shah,P.Sharma,J.V.Shah,et al.,An improved LC-MS/MS method for the simultaneous determination of pyrazinamide,pyrazinoic acid and 5-hydroxy pyrazinoic acid inhuman plasma for a pharmacokinetic study,J.Chromatogr.B1017(2016)52-61.
[18]Guidance for Industry:ICH E6 Good Clinical Practice.US.Department of Health and Human Services,Food and Drug Administration,Centre for Drug Evaluation and Research(CDER),Centre for Biologies Evaluation and Research(CBER).1996.
[19]M.Yadav,P.S.Shrivastav,Incurred sample reanalysis(ISR):a decisive tool in bioanalytical research,Bioanalysis 3(2011)1007-1024.