Research Journal of Pharmacy and Technology

Open Access Open Access  Restricted Access Subscription Access
Open Access Open Access Open Access  Restricted Access Restricted Access Subscription Access

Stability Indicating RP-HPLC Method for the Estimation of Emtricitabine and Tenofovir Disoproxil Fumerate in Tablet Dosage Form


Affiliations
1 Department of Pharmaceutical Analysis, The Erode College of Pharmacy and Research, Erode- 638112, India
     

   Subscribe/Renew Journal


A simple, accurate and precise reverse phase high performance liquid chromatographic (RP-HPLC) method was developed for the simultaneous quantitative estimation of Emtricitabine (EMT) and Tenofovir disoproxil fumerate (TDF) in tablet dosage form. Quantitation was carried on an ACE (150 mm x 4.6mm, 5μ) column using gradient composition of 0.01 M citric acid monohydrate buffer pH 4.5 as mobile phase A and methanol as mobile phase B at a flow rate of 1.0 mL/min with detection at 260 nm. Determination of the different validation parameters such as precision, linearity, accuracy, specificity, robustness, limit of detection, limit of quantification and filter validation was done. The system suitability parameters such as retention time, theoretical plates and tailing factor were found to be 3.181min, 13438, 0.14 and 6.090min, 48847, 1.05 respectively for EMT and TDF. The detector response is linear from 16 μg/mL to 64 μg/mL for EMT and 24 μg/mL to 96 μg/mL TDF. The limit of detection and limit of quantification was 0.101, 0.189 μg/mLand 0.306, 0.575 μg/mL for EMT and TDF respectively. The percentage recovery for average of three different concentrations (50, 100 and 150%) was 101.1, 100.6, 99.8 and 99.7, 99.4, 99.6% for EMT and TDF respectively.The high percentage of recovery and low % RSD confirms the suitability of the method for the simultaneous estimation of EMT and TDF in tablet dosage form.The method could effectively separate the drugs from their degradation products, it can be regarded as stability indicating method.

Keywords

RP-HPLC, Simultaneous Estimation, EMT, TDF, Forced Degradation Studies
Subscription Login to verify subscription
User
Notifications
Font Size


  • www.drugbank.com

  • Appala NR, Rao VJ, Vanitha PK, Mukilteo K and Srinivasu K. Simultaneous estimation of tenofovir disoproxil, emtricitabine and efavirenz in tablet dosage form by RP- HPLC. Orient J Chem. 24(2); 2008: in press.

  • Appala Raju N and Shabana Begum. Simultaneous RP-HPLC method for the estimation of the emtricitabine, tenofovir disoproxil fumerate and efavirenz in tablet dosage forms. Research Journal of Pharmacy and Technology. 1(4); 2008: 522-525.

  • Shirkhedkar AA, Bhirud CH and Surana SJ. Application of UV spectrophotmetric methods for estimation of tenofovir disoproxil fumarate in tablets. Pak. J. Pharm. Sci. 22(1); 2009: 27-29.

  • Sparidans RW, Crommentuyn KML, Schellens JHM and Beijnen JH. Liquid chromatographic assay for the antiviral nucleotide analogue tenofovir in plasma using derivatization with chloroacetaldehyde. Journal of Chromatography B. 791 (1-2); 2003: 227–233.

  • Sentenac S, Fernandez C, Thuillier A, Lechat P and Aymard G. Sensitive determination of tenofovir in human plasma samples using reversed-phase liquid chromatography. Journal of ChromatographyB. 793 (2); 2003: 317–324.

  • Kandagal PB, Manjunatha DH and Seetharamappa J. RP-HPLC Method for the determination of tenofovir in pharmaceutical formulations and spiked human plasma. Analytical letters. 41(4); 2008: 561-570.

  • Delahunty T, Bushman L and Fletcher CV. Sensitive assay for determining plasma Tenofovir concentrations by LC/MS/MS. Journal of Chromatography B. 830; 2006: 6–12

  • Masaaki T,Yuichi K, Naoya O, Atsushi H, Kazuhide B and Tsuguhiro K. Determination of plasma tenofovir concentrations using a conventional LC-MS method. Biological & Pharmaceutical Bulletin. 30; 2007:1784.

  • King T, Bushman L, Kiser J, Anderson PL, Ray M, Delahunty T and Fletcher CV. Liquid chromatography tandem mass spectrometric determination of tenofovir diphosphate in human peripheral blood mononuclear cells. Journal of ChromatographyB. 843 (2); 2006: 147–156.

  • Droste JAH, Aarnoutse RE and Burger DM. Determination of emtricitabine in human plasma using HPLC with fluorometric detection. Journal of Liquid Chromatography & Related Technologies. 30 (18); 2007: 2769 – 2778.

  • Unnam S, Bodepudi H, Kottapalli B and Chandrasekhar. Development and validation of a stability-indicating liquid chromatographic method for determination of emtricitabine and related impurities in drug substance. Journal of Separation Science. 30; 2007:999 – 1004

  • Rezk NL,Crutchley RD, Kashuba ADM. Simultaneous quantification of emtricitabine and tenofovir in human plasma using high performance liquid chromatography after solid phase extraction. Journal of Chromatography B. 822; 2005: 201.

  • Gomes NA, Vaidya VV, Pudage A, Joshi SS, Parekh SA. Liquid chromatography–tandem mass spectrometry (LC–MS/MS) method for simultaneous determination of tenofovir and emtricitabine in human plasma and its application to a bioequivalence study. Journal of Pharmaceutical and Biomedical Analysis. 48; 2008: 918–926.

  • Maithilee Joshi, Nikalje AP, Shahed M and Dehghan M. HPTLC method for the simultaneous estimation of emtricitabine and tenofovir in tablet dosage form. Indian Journal of Pharmaceutical Sciences. 71(1); 2009: 95–97.


Abstract Views: 787

PDF Views: 0




  • Stability Indicating RP-HPLC Method for the Estimation of Emtricitabine and Tenofovir Disoproxil Fumerate in Tablet Dosage Form

Abstract Views: 787  |  PDF Views: 0

Authors

K. Shailaja
Department of Pharmaceutical Analysis, The Erode College of Pharmacy and Research, Erode- 638112, India
R. Revathi
Department of Pharmaceutical Analysis, The Erode College of Pharmacy and Research, Erode- 638112, India
V. S. Saravanan
Department of Pharmaceutical Analysis, The Erode College of Pharmacy and Research, Erode- 638112, India

Abstract


A simple, accurate and precise reverse phase high performance liquid chromatographic (RP-HPLC) method was developed for the simultaneous quantitative estimation of Emtricitabine (EMT) and Tenofovir disoproxil fumerate (TDF) in tablet dosage form. Quantitation was carried on an ACE (150 mm x 4.6mm, 5μ) column using gradient composition of 0.01 M citric acid monohydrate buffer pH 4.5 as mobile phase A and methanol as mobile phase B at a flow rate of 1.0 mL/min with detection at 260 nm. Determination of the different validation parameters such as precision, linearity, accuracy, specificity, robustness, limit of detection, limit of quantification and filter validation was done. The system suitability parameters such as retention time, theoretical plates and tailing factor were found to be 3.181min, 13438, 0.14 and 6.090min, 48847, 1.05 respectively for EMT and TDF. The detector response is linear from 16 μg/mL to 64 μg/mL for EMT and 24 μg/mL to 96 μg/mL TDF. The limit of detection and limit of quantification was 0.101, 0.189 μg/mLand 0.306, 0.575 μg/mL for EMT and TDF respectively. The percentage recovery for average of three different concentrations (50, 100 and 150%) was 101.1, 100.6, 99.8 and 99.7, 99.4, 99.6% for EMT and TDF respectively.The high percentage of recovery and low % RSD confirms the suitability of the method for the simultaneous estimation of EMT and TDF in tablet dosage form.The method could effectively separate the drugs from their degradation products, it can be regarded as stability indicating method.

Keywords


RP-HPLC, Simultaneous Estimation, EMT, TDF, Forced Degradation Studies

References