BIO-ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF FINASTERIDE, TADALAFIL, AND ITS APPLICATION TO PHARMACOKINETIC STUDIES IN RAT PLASMA BY USING LC-MS/MS

YESUPADAMU RAYINUTHALA; DAVID RAJU MEDEPALLI; A. LAKSHMANARAO

doi:10.22159/ijap.2024v16i5.50858

Authors

YESUPADAMU RAYINUTHALA Department of Chemistry, Government Degree College, Chebrole, Guntur District, AP-522212, India
DAVID RAJU MEDEPALLI Department of Chemistry, P B Siddhartha College of Arts and Science, Mogalraj Puram, Vijayawada, AP, India
A. LAKSHMANARAO Department of Chemistry, Sri ABR Government Degree College, Repalle, Bapatla District, AP-522265, India

DOI:

https://doi.org/10.22159/ijap.2024v16i5.50858

Keywords:

Finasteride, Tadalafil, LC-MS/MS, USFDA guidelines, Rat plasma

Abstract

Objective: An easy, quick, precise, active and reproducible LC-MS/MS (Liquid Chromatography Tandem Mass Spectrometry) technique was developed for the bio-analytical method of Finasteride and Tadalafil using Avanafil as internal standard (IS).

Methods: This article summarizes the recent progress on bioanalytical liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS) methods using waters Symmetry C₁₈ column (150x4.6 mm, 3.5µ) column and mobile phase of 0.1% Perchloric acid and Acetonitrile (ACN) in 60:40.

Results: The calibration curve was linear in the range of 12.5-100 ng/ml for Finasteride and 12.5-100 ng/ml Tadalafil. The recovery results of Accuracy and Precision of Finasteride and Tadalafil were 95.10, 96.85, 98.76, 98.81% and 95.77, 97.46, 97.99, 97.01% at different QC (Quality Control) concentration levels. Matrix effect results were within the acceptable limit. An electro-spray ionization source was used to study of Finasteride and Tadalafil at m/z 373.5497→142.0085, m/z 390.4047→128.1138 for Finasteride and Tadalafil, m/z 484.9516→104.5326 for Avanafil were ion pairs of mass analysis.

Conclusion: The application denotes all the parameters of system suitability, specificity, linearity and accuracy are in good agreement with USFDA (United States of Food and Drug Administration) guidelines and applied effectively for the investigation of pharmacokinetic studies in rat.

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References

Silva V, Grande AJ, Peccin MS. Physical activity for lower urinary tract symptoms secondary to benign prostatic obstruction. Cochrane Database Syst Rev. 2019;4(4):CD012044. doi: 10.1002/14651858.CD012044.pub2, PMID 30953341.

Hwang EC, Gandhi S, Jung JH, Imamura M, Kim MH, Pang R. Naftopidil for the treatment of lower urinary tract symptoms compatible with benign prostatic hyperplasia. Cochrane Database Syst Rev. 2018;10(10):CD007360. doi: 10.1002/14651858.CD007360.pub3, PMID 30306544.

Keehn A, Taylor J, Lowe FC. Phytotherapy for benign prostatic hyperplasia. Curr Urol Rep. 2016;17(7):53. doi: 10.1007/s11934-016-0609-z, PMID 27180172.

McNicholas TA. Benign prostatic hyperplasia and new treatment options-a critical appraisal of the UroLift system. Med Devices (Auckl). 2016;9:115-23. doi: 10.2147/MDER.S60780, PMID 27274321.

Knezevich EL, Viereck LK, Drincic AT. Medical management of adult transsexual persons. Pharmacotherapy. 2012;32(1):54-66. doi: 10.1002/PHAR.1006, PMID 22392828.

Morinaga H, Mohri Y, Grachtchouk M, Asakawa K, Matsumura H, Oshima M. Obesity accelerates hair thinning by stem cell-centric converging mechanisms. Nature. 2021;595(7866):266-71. doi: 10.1038/s41586-021-03624-x, PMID 34163066.

Ramos PM, Miot HA. Female pattern hair loss: a clinical and pathophysiological review. An Bras Dermatol. 2015;90(4):529-43. doi: 10.1590/abd1806-4841.20153370, PMID 26375223.

Polak Witka K, Rudnicka L, Blume Peytavi U, Vogt A. The role of the microbiome in scalp hair follicle biology and disease. Exp Dermatol. 2020;29(3):286-94. doi: 10.1111/exd.13935, PMID 30974503.

Matsumura H, Mohri Y, Binh NT, Morinaga H, Fukuda M, Ito M. Hair follicle aging is driven by transepidermal elimination of stem cells via COL17A1 proteolysis. Science. 2016;351(6273):aad4395. doi: 10.1126/science.aad4395, PMID 26912707.

Nomani H, Mohammadpour AH, Moallem SM, YazdanAbad MJ, Barreto GE, Sahebkar A. Anti-androgen drugs in the treatment of obsessive-compulsive disorder: a systematic review. Curr Med Chem. 2020;27(40):6825-36. doi: 10.2174/0929867326666191209142209, PMID 31814547.

Zorumski CF, Paul SM, Covey DF, Mennerick S. Neurosteroids as novel antidepressants and anxiolytics: GABA-A receptors and beyond. Neurobiol Stress. 2019;11:100196. doi: 10.1016/j.ynstr.2019.100196, PMID 31649968.

Reddy DS, Estes WA. Clinical potential of neurosteroids for CNS disorders. Trends Pharmacol Sci. 2016;37(7):543-61. doi: 10.1016/j.tips.2016.04.003, PMID 27156439.

Morrow AL, Boero G, Porcu P. A rationale for allopregnanolone treatment of alcohol use disorders: basic and clinical studies. Alcohol Clin Exp Res. 2020;44(2):320-39. doi: 10.1111/acer.14253, PMID 31782169.

Wang Y, Bao Y, Liu J, Duan L, Cui Y. Tadalafil 5 mg once daily improves lower urinary tract symptoms and erectile dysfunction: a systematic review and meta-analysis. Low Urin Tract Symptoms. 2018;10(1):84-92. doi: 10.1111/luts.12144, PMID 29341503.

Qato DM, Wilder J, Schumm LP, Gillet V, Alexander GC. Changes in prescription and over-the-counter medication and dietary supplement use among older adults in the United States, 2005 vs 2011. JAMA Intern Med. 2016;176(4):473-82. doi: 10.1001/jamainternmed.2015.8581, PMID 26998708.

Humbert M, Kovacs G, Hoeper MM, Badagliacca R, Berger RM, Brida M. ESC/ERS guidelines for the diagnosis and treatment of pulmonary hypertension. Eur Heart J. 2022;43(38):3618-731. doi: 10.1093/eurheartj/ehac237, PMID 36017548.

Bordones Crom A, Patnaik SS, Menon PG, Murali S, Finol E. Morphological analysis of the right ventricular endocardial wall in pulmonary hypertension. J Biomech Eng. 2021;143(7). doi: 10.1115/1.4050457, PMID 33704381.

Mouratoglou SA, Bayoumy AA, Noordegraaf AV. Prediction models and scores in pulmonary hypertension: a review. Curr Pharm Des. 2021;27(10):1266-76. doi: 10.2174/1381612824999201105163437, PMID 33155897.

Petersen KS, Kris Etherton PM. Diet quality assessment and the relationship between diet quality and cardiovascular disease risk. Nutrients. 2021;13(12):4305. doi: 10.3390/nu13124305, PMID 34959857.

Semsarian C, Ingles J, Ross SB, Dunwoodie SL, Bagnall RD, Kovacic JC. Precision medicine in cardiovascular disease: genetics and impact on phenotypes: JACC focus seminar 1/5. J Am Coll Cardiol. 2021;77(20):2517-30. doi: 10.1016/j.jacc.2020.12.071, PMID 34016265.

Sola J, Bertschi M, Krauss J. Measuring pressure: introducing oBPM, the optical revolution for blood pressure monitoring. IEEE Pulse. 2018;9(5):31-3. doi: 10.1109/MPUL.2018.2856960, PMID 30273141.

Chandrasekhar A, Kim CS, Naji M, Natarajan K, Hahn JO, Mukkamala R. Smartphone-based blood pressure monitoring via the oscillometric finger-pressing method. Sci Transl Med. 2018;10(431):eaap8674. doi: 10.1126/scitranslmed.aap8674, PMID 29515001.

Abdelazim AH, Ramzy S. Simultaneous spectrophotometric determination of finasteride and tadalafil in recently FDA approved Entadfi™ capsules. BMC Chem. 2022;16(1):55. doi: 10.1186/s13065-022-00850-w, PMID 35906639.

Pappula N, Kodali B, Datla PV. Selective and rapid determination of tadalafil and finasteride using solid phase extraction by high performance liquid chromatography and tandem mass spectrometry. J Pharm Biomed Anal. 2018;152:215-23. doi: 10.1016/j.jpba.2018.01.020, PMID 29427880.

Kammoun AK, Khayat MT, Almalki AJ, Youssef RM. Development of validated methods for the simultaneous quantification of finasteride and tadalafil in newly launched FDA-approved therapeutic combination: greenness assessment using AGP, analytical eco-scale, and GAPI tools. RSC Adv. 2023;13(17):11817-25. doi: 10.1039/D3RA01437A, PMID 37077997.

Ramadevi P, Rambabu K. Bioanalytical method development and validation for ezetimibe and pitavastain and its applications to pharmacokinetic studies in Rabbit plasma by using LCMS/MS. IJRPS. 2020;11(4):7854-62. doi: 10.26452/ijrps.v11i4.4670.

Eluru A, Surendra Babu K. Bioanalytical method development and validation for aplidine in rat plasma and their pharmacokinetic studies by LCMS. WJPPS. 2019;8:1201-9.

Ramchandran D, Kethipalli A, Krishnamurthy M. Bio-analytical method development and validation of daunorubicin and cytrarabine in rat plasma by LC-MS/MS and its application in pharmacokinetic studies. J Pharm Sci Res. 2020;12:381-6.

Naykode MD, Bhagwat DA, Jadhav SD, More HN. Analytical and bioanalytical method for quantification of pure azilsartan, not its salts by RP-HPLC. Res J Pharm Technol. 2017;10(3):708-14. doi: 10.5958/0974-360X.2017.00133.0.

Singh M, Charde M, Shukla R, Rita MC. Determination of calcipotriene in calcipotriene cream 0.05% w/w by RP-HPLC method development and validation. Res J Pharm Technol. 2011;4:1219-23.

Malathi S, Arunadevi N. Development and validation of stability-indicating simultaneous estimation of metformin and alogliptin in tablets by high-performance thin layer chromatography. Int J Pharm Pharm Sci. 2020;12:68-73.

Senthil Rajan D, Muruganathan G, Shivkumar K, Ganesh T. Development and validation of HPLC method for simultaneous quantification of vasicine, glycyrrhizin and piperine in polyherbal cough syrup. Int J Curr Pharm Res. 2020;12:15-9.

Shanmugasundaram P, Kamarapu SK. RP-HPLC method for the simultaneous estimation and validation of amlodipine besylate and atenolol in bulk and tablet dosage form in biorelevant dissolution medium (Fassif). Res J Pharm Technol. 2017;10(10):3379-85. doi: 10.5958/0974-360X.2017.00601.1.

Gomathy S, Narenderan ST, Meyyanathan SN, Gowramma B. Development and validation of HPLC method for the simultaneous estimation of apigenin and luteolin in commercial formulation. J Crit Rev. 2020;7:4785-90.

kumar SA, Debnath Anidipa, Rao JV, Sankar DG. Development and validation of a sensitive RP-HPLC method for simultaneous estimation of rosuvastatin and fenofibrate in tablet dosage form by using PDA detector in gradient mode. Res J Pharm Technol. 2016;9(5):549-54. doi: 10.5958/0974-360X.2016.00104.9.

Malak Y, Al-Bathish AA, Gazy MK, El-Jamal. RP-HPLC and chemometric methods for the determination of two antidiabetic mixtures; metformin hydrochloride-canagliflozin and metformin hydrochloride-gliclazide in their pharmaceutical formulation. Int J Pharm Pharm Sci. 2020;12:83-94.

Gadhvi MP, Bhandari A, Suhagia BN, Desai UH. Development and validation of RP-HPLC method for simultaneous estimation of atazanavir and ritonavir in their combined tablet dosage form. Res J Pharm Technol. 2013;6:200-3.

Koya Prabhakara Rao Nl, A Amara Babu, Kalyani Koganti, Babji Palakeeti, Koduri SV Srinivas. Related substances method development and validation of an LC-MS/MS method for the quantification of selexipag and its related impurities in rat plasma and its application to pharmacokinetic studies. SN Appl Sci. 2021;3:321.

Hasanah YI, Harahap Y, Suryadi H. Development and validation method of cyclophosphamide and 4-hydroxy cyclophosphamide with 4-hydroxy cyclophosphamide-D4 as internal standard in dried blood spots using UPLC-MS/MS. Int J Appl Pharm. 2021;13:148-52.

Naveen VM, Veeraswami B, Srinivasa Rao G. High response bio-analytical validation approach of nadolol and Bendroϑlumethiazide by LC-MS/MS on rat plasma. IJRPS. 2020;11(SPL4):2272-9. doi: 10.26452/ijrps.v11iSPL4.4454.

Kumari GK, Kantipudi R. Bio analytical method development and validation for Avapritinib in rat plasma by LC-MS/MS. J Pharm Sci Res. 2021;13:134-7.

Hemanth Kumar AK, Sudha V, Vijayakumar A, Padmapriyadarsini C. Simultaneous method for the estimation of bidaquiline and delamanid in human plasma using high performance liquid chromatography. Int J Pharm Pharm Sci. 2021;13:36-40.

Chaitanya SM, Nissankararao S, Gandham S. A sort of validated bioanalytical method developed for the estimation of etoposide and cisplatin in rat plasma by using two different advanced liquid chromatographic techniques like HPLC and UPLC and its application in bioequivalence studies. IJRPS. 2021;12(1):708-17. doi: 10.26452/ijrps.v12i1.4167.

Sura RS, Cvs S, Rachamalla SS. Bioanalytical RP-HPLC method development and validation of clopidogrel bisulfate in wistar rat plasma and its application to pharmacokinetic study. Int J App Pharm. 2022;14:106-11. doi: 10.22159/ijap.2022v14i1.43328.

Thomas A, Varkey J. Development and validation of a new RP-HPLC analytical method for the determination of etodolac succinic acid co. crystals in spiked rabbit plasma. Int J Curr Pharm Sci. 2023;15:59-63. doi: 10.22159/ijcpr.2023v15i2.2098.

Shah SK, Dey S, De S. Simultaneous determination of atorvastatin and atenolol in rabbit plasma by RP-HPLC method and its application in pharmacokinetic study. Int J Curr Pharm Sci. 2022;14:72-8. doi: 10.22159/ijcpr.2022v14i2.1968.

Sunder BS, Mittal AK. Bio-analytical method development and validation for simultaneous determination of ledipasvir and sofosbuvir drugs in human plasma by RP-HPLC method. Int J Curr Pharm Sci. 2018;10(3):21-6. doi: 10.22159/ijcpr.2018v10i3.27223.

Kulkarni DC, Dadhich AS, Annapurna MM. Method development and validation of a new stability indicating HPLC and LC-APCI-MS methods for the determination of bumetanide. Res J Pharm Technol. 2023;16:3809-7.

Saurav R, Derle DD, Wakchaure AA, Amrutkar AA, More AV. Development and validation of bio-analytical method for the estimation of Rivaroxaban using RP-HPLC with liquid extraction in human blood plasma and its application in bioequivalence study. Res J Pharm Technol. 2024;17:739-5.

Tamilselvi N, Kanagapriya K. Bioequivalence study and bioanalytical method development of Remogliflozin etabonate tablets in wistar rat plasma using RP-HPLC method. Res J Pharm Technol. 2024;17:789-94. doi: 10.52711/0974-360X.2024.00122.

Marakatham S, Shanmugapandiyan P. Stability indicating bioanalytical validation of elexacaftor, ivacaftor and tezacaftor using HPLC in human plasma. Res J Pharm Technol. 2023;16:3780-6. doi: 10.52711/0974-360X.2023.00624.

Yamani NS, Mathrusri Annapurna M, Raj Kumar PV. A new stability indicating HPLC and LC-APCI-MS methods for the estimation of dacomitinib in pharmaceutical dosage forms. Res J Pharm Technol. 2023;16:4391-8. doi: 10.52711/0974-360X.2023.00718.

Eluru J, Mathrusri Annapurna MA. A new stability indicating HPLC and LC-APCI-MS methods for the estimation of flucytosine in pharmaceutical dosage forms. Res J Pharm Technol. 2023;16:5296-302. doi: 10.52711/0974-360X.2023.00858.

Anusha Venna RS, Koppala RVSC, Aleti R, Ramana Murthy Kolapalli V. Bioanalytical method for the preclinical estimation of donepezil hydrochloride in rabbit plasma by RP-HPLC. Res J Pharm Technol. 2023;16:5207-2.

Vaka PR, Battula SR. Sensitive and rapid LCMS/MS method for the estimation of recently approved antiviral drugs maribavir and fostemsavir in spiked human plasma. Res J Pharm Technol. 2023;16:5149-4.

Jabeen SBV. Simultaneous determination of cefepime and tazobactam by using hyphenated liquid chromatography. Res J Pharm Technol. 2024;17:67-3.

Manoranjani M. LC-MS/MS method for simultaneous estimation of ethinyl estradiol and etonogestrel in rat plasma and its application to pharmacokinetic study. High Technol Lett. 2023;29:543-56.

Satyadev TN, Uma Mahesh A, Durga Bhavani N, Rohith M. High performance liquid chromatographic-mass spectrometric method for development and validation of belzutifan in rat plasma. High Technol Lett. 2023;29:640-54.

Baje Syed IB, Nannapaneni M. Bio analytical validation method for capmatinib and spartalizumab in rabbit plasma by using highly effective mass spectrophotometric method. Rasayan J Chem. 2022;15(4):2748-55. doi: 10.31788/RJC.2022.1547098.

Prasanthi S, Himabindu G. Bioanalytical method for simultaneous estimation of ezetimibe and pitavastatin and its application to pharmacokinetic studies using UPLC. Ymer. 2022;21(2):718-32. doi: 10.37896/YMER21.02/67.

Prasanthi S, Himabindu G. Assay of bioanalytical method for the estimation of avelumab and axitinib using UPLC and its application to pharmacokinetic studies. JPRI. 2022;34:1-10. doi: 10.9734/jpri/2022/v34i27A35988.

Kantipudi R, Pavuluri SK. Bioanalytical method development and validation for the simultaneous estimation of olanzapine and samidorphan in rabbit plasma by using HPLC–MS/MS and application to pharmacokinetic study. Futur J Pharm Sci. 2024;10(1):1-14. doi: 10.1186/s43094-023-00570-5.

Rathore MK, Mohan Reddy TR. Tandem mass spectrometric method for the trace level determination of 2-aminopyridine: a potential genotoxic impurity in tenoxicam API. Int J Pharm Pharm Sci. 2024;16:50-6. doi: 10.22159/ijpps.2024v16i4.49902.

Gurav P, Damle M. Bioanalytical method for estimation of teriflunomide in human plasma. Int J Pharm Pharm Sci. 2022;14:19-23.

Elham G, Sima S, Javad S, Shahram S. Analytical method validation, pharmacokinetic and bioequivalence study of dimethyl fumarate in healthy Iranian volunteers. Int J Pharm Pharm Sci. 2021;13:6-10. doi: 10.22159/ijpps.2021v13i9.42328.

Hemanth Kumar AK, Sudha V, Vijaya Kumar A, Padmapriyadarsini P. Simultaneous method for the estimation of bedaquiline and delamanid in Human Plasma using high-performance liquid chromatography. Int J Pharm Pharm Sci. 2021;13:36-40.

Sellappan M, Devakumar D. Development and validation of RP-HPLC method for the estimation of escitalopram oxalate and flupentixol dihydrochloride in combined dosage form and plasma. Int J Pharm Pharm Sci. 2021;13:61-6. doi: 10.22159/ijpps.2021v13i2.30158.

Halder D, Das S, Ghosh B, Biswas E. An LC-MA/MS based bio analytical approach to resolve pharmacokinetic investigation of acotiamide hydrochloride and its application to a bioequivalence study. Int J Pharm Pharm Sci. 2020;12:76-84.

Korake S, Pawar A, Surywanshi S, Bothiraja C, Pawar A. High performance liquid chromatography for the simultaneous estimation of cefoperazone and sulbactam in rat plasma and its importance in therapeutic drug monitoring. Int J Pharm Pharm Sci. 2020;12:92-7. doi: 10.22159/ijpps.2020v12i10.38638.

Kantipudi R, Pavuluri SK. Bioanalytical method development and validation for the simultaneous estimation of olanzapine and samidorphan in rabbit plasma by using HPLC–MS/MS and application to pharmacokinetic study. Futur J Pharm Sci. 2024;10(1):1-14. doi: 10.1186/s43094-023-00570-5.

Talari S, Vejendla A, Shetty RK. Development and validation of a UPLC-MS/MS method for the simultaneous determination of verapamil and trandolapril in rat plasma: application to a pharmacokinetic study. Curr Pharm Anal. 2022;18(3):291-304. doi: 10.2174/1573412917666210302145711.

Talari S, Vejendla A, Boddapati SN, Kalidindi J. LC-MS/MS method development and validation of lenvatinib and its related impurities in rat plasma: application to a pharmacokinetic study. Curr Pharm Anal. 2022;18(6):614-28. doi: 10.2174/1573412918666220330004440.

Yarlagadda SR, Pavani Y, Mannam SR. Simultaneous method development and validation of trastuzumab and hyaluronidase-risk and its pharmacokinetic studies with LC-MS/MS. J Pharm Sci Res. 2020;12:375-80.