Multivariate optimization and validation of an analytical methodology by RP-HPLC for the determination of losartan potassium in capsules

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)This paper describes the optimization and validation of an analytical methodology for the determination of losartan potassium in capsules by HPLC using 2(5-1) fractional factorial and Doehlert designs. This multivariate approach allows a considerable improvement in chromatographic performance using fewer experiments, without additional cost for columns or other equipment. The HPLC method utilized potassium phosphate buffer (pH 6.2: 58 mmol L(-1))-acetonitrile (65:35, v/v) as the mobile phase, pumped at a flow rate of 1.0 mL min(-1). An octylsilane column (100 mm x 4.6 mm W., 5 mu m) maintained at 35 degrees C was used as the stationary phase. UV detection was performed at 254 nm. The method was validated according to the ICH guidelines, showing accuracy, precision (intra-day relative standard deviation (R.S.D.) and inter-day R.S.D values <2.0%). selectivity, robustness and linearity (r=0.9998) over a concentration range from 30 to 70 mg L(-1) of losartan potassium. The limits of detection and quantification were 0.114 and 0.420 mg L(-1), respectively. The validated method may be used to quantify losartan potassium in capsules and to determine the stability of this drug. (C) 2009 Elsevier B.V. All rights reserved.801236241Center of Pharmaceutical Equivalence of the Federal University of AlfenasFederal University of AlfenasConselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq

Multivariate Optimization And Validation Of An Analytical Methodology By Rp-hplc For The Determination Of Losartan Potassium In Capsules

This paper describes the optimization and validation of an analytical methodology for the determination of losartan potassium in capsules by HPLC using 25-1 fractional factorial and Doehlert designs. This multivariate approach allows a considerable improvement in chromatographic performance using fewer experiments, without additional cost for columns or other equipment. The HPLC method utilized potassium phosphate buffer (pH 6.2; 58 mmol L-1)-acetonitrile (65:35, v/v) as the mobile phase, pumped at a flow rate of 1.0 mL min-1. An octylsilane column (100 mm × 4.6 mm i.d., 5 μm) maintained at 35 °C was used as the stationary phase. UV detection was performed at 254 nm. The method was validated according to the ICH guidelines, showing accuracy, precision (intra-day relative standard deviation (R.S.D.) and inter-day R.S.D values &lt;2.0%), selectivity, robustness and linearity (r = 0.9998) over a concentration range from 30 to 70 mg L-1 of losartan potassium. The limits of detection and quantification were 0.114 and 0.420 mg L-1, respectively. The validated method may be used to quantify losartan potassium in capsules and to determine the stability of this drug. © 2009 Elsevier B.V. All rights reserved.801236241The United States Pharmacopoeia, 31st ed., United States Pharmacopoeial Convection, Rockville, MD, 2008, p. 2554Barreiro, E.J., Fraga, C.A.M., (2001) Química Medicinal: As bases moleculares da ação dos fármacos, p. 97. , Artmed, São Paulo/Porto AlegreSchoenberger, J.A., (1995) J. Hypertens., 13, pp. S43-S47Williams, R.C., Alasandro, M.S., Fasone, V.L., Boucher, R.J., Edwards, J.F., (1996) J. Pharm. Biomed. Anal., 14, pp. 1539-1546Furtek, C.I., Lo, M.W., (1992) J. Chromatogr., 573, pp. 295-301Kristoffersen, L., Øiestad, E.L., Opdal, M.S., Krogh, M., Lundanes, E., Christophersen, A.S., (2007) J. Chromatogr. B, 850, pp. 147-160Lee, H., Shim, H.O., Lee, H.S., (1996) Chromatographia, 42, pp. 39-42Yeung, P.K., Jamieson, A., Smith, G.J., Fice, D., Pollak, P.T., (2000) Int. J. Pharm., 204, pp. 17-22Ansari, M., Kazemipour, M., Khosravi, F., Baradaran, M., (2004) Chem. Pharm. Bull., 52, pp. 1166-1170Carlucci, G., Palumbo, G., Mazzeo, P., Quaglia, M.G., (2000) J. Pharm. Biomed. Anal., 23, pp. 185-189Erk, N., (2001) J. Pharm. Biomed. Anal., 24, pp. 603-611Hertzog, D.L., McCafferty, J.F., Fang, X., Tyrrell, R.J., Reed, R.A., (2002) J. Pharm. Biomed. Anal., 30, pp. 747-760Lusina, M., Cindri'c, T., Tomai'c, J., Peko, M., Pozai'c, L., Musulin, N., (2005) Int. J. Pharm., 291, pp. 127-137Obando, M.A., Estela, J.M., Cerda, V., (2008) Anal. Bioanal. Chem., 391, pp. 2349-2356Seburg, R., Ballard, J.M., Hwang, T., Sullivan, C.M., (2006) J. Pharm. Biomed. Anal., 42, pp. 411-422Sreekanth, N., Shivshanker, K., Shanmuga Pandian, P., Roosewelt, C., Srinivasa Rao, G., Gunasekaran, V., (2007) Asian J. Chem., 19, pp. 2850-2856Zhao, Z., Wang, Q., Tsai, E., Qin, X., Ip, X.D., (1999) J. Pharm. Biomed. Anal., 20, pp. 129-136Maio, V.M.P., Dias, C.L., Bergold, A.M., (2005) Acta Farm. Bonaerense, 24, pp. 250-255McCarthy, K.E., Wang, Q., Tsai, E.W., Gilbert, R.E., Ip, D.P., Brooks, M.A., (1998) J. Pharm. Biomed. Anal., 17, pp. 671-677Sathe, S.R., Bari, S.B., (2007) Acta Chromatogr., 19, pp. 270-278Quaglia, M.G., Donati, E., Carlucci, G., Mazzeo, P., Fanali, S., (2002) J. Pharm. Biomed. Anal., 29, pp. 981-987Lastra, O.C., Lemus, I.G., Sánchez, H.J., Pérez, R.F., (2003) J. Pharm. Biomed. Anal., 33, pp. 175-180Maggio, R.M., Castellano, P.M., Kaufman, T.S., (2008) Anal. Bioanal. Chem., 391, pp. 2949-2955Prabhakar, A.H., Giridhar, R., (2002) J. Pharm. Biomed. Anal., 27, pp. 861-866Choi, Y., Liq, J., (2008) Chromatogr. Rel. Technol., 31, pp. 2643-2656Neves, R., (2008) Arzneim. Forsch., 58, pp. 369-375Ferreira, S.L.C., Santos, W.N.L., Quintella, C.M., Neto, B.B., Bosque-Sendra, J.M., (2004) Talanta, 63, pp. 1061-1067Montgomery, D.C., (2000) Design, Analysis of Experiments, , Wiley, New York pp. 177-185International Conference on Harmonization of Technical Requirements for the Registration of Pharmaceutical for Human Use: Validation of Analytical Procedures, Text and Methodology, Q2 R1, 2005Center for Drug Evaluation and Research (CDER) Validation of Chromatographic Methods, Reviewer Guidance, obtained from web site, , http://www.fda.gov/CDER/GUIDANCE/cmc3.pdfTzanavaras, P.D., Themelis, D.G., Zotou, A., Stratis, J., Karlberg, B., (2008) J. Pharm. Biomed. Anal., 46, pp. 670-67

QUALITY CONTROL OF HYDROCHLOROTHIAZIDE TABLETS MARKETED IN SINOP-MT

The thiazide diuretics are of the classes of drugs most frequently used for the treatment of hypertension. Hydrochlorothiazide is the representative of this class and is found in tablet form in doses of 25 and 50 mg. It is marketed in three different categories of drugs: reference, similar and generic. According to the regulator in Brazil, the National Health Surveillance Agency (ANVISA), before pharmaceuticals are released for use, the pharmaceutical industry must meet product quality specifications, but the consumption of counterfeit drugs, contraband or without registration with government laws It is growing in Brazil, which affect the entire drug production chain affecting the health of those who use these medicines. In view of the reported problems about the quality of marketed drugs and being the state of Mato Grosso considered a fake gateway drug, due to its proximity to Bolivia, this study aimed to assess the quality of tablets containing hydrochlorothiazide is already one of the most widely used drugs in the treatment of hypertension in Sinop-MT municipality according local search. Samples from five laboratories that produce hydrochlorothiazide tablets at a dose of 25 mg, and the most market in the municipality of Sinop / MT were analyzed as stablished in the Brazilian Pharmacopoeia. It was found that four of the five samples of drugs in Mato Grosso, performed all the requirements for approval in quality testing, with the exception of a product that has lower hardness values than recommended, which can lead to problems drug presentation as well as directly affect the absorption, bioavailability and action of the therapeutic drug. It was concluded that medicinal products containing hydrochlorothiazide showed adequate quality, ensuring their effectiveness

Multivariate Development and Validation of a Stability-Indicating HPLC Method for the Determination of Glimepiride in Tablets

This paper describes the multivariate development of a stability-indicating HPLC method for the quantification of glimepiride in pharmaceutical tablets. Full factorial design, Doehlert design, and response-surface methodology were used in conjunction with the desirability function approach. This procedure allowed the adequate separation of glimepiride from all degradant peaks in a short analysis time (about 9 min). This HPLC method uses potassium phosphate buffer (pH 6.5; 27.5 mmol/L)-methanol (34 + 66, v/v) mobile phase at a flow rate of 1.0 mL/min and UV detection at 228 nm. A Waters Symmetry (R) C18 column (250 x 4.6 mm, 5.0 mu m) at controlled room temperature (25 degrees C) was used as the stationary phase. The method was validated according to International Conference on Harmonization guidelines and demonstrated linearity from 2 to 40 mg/L glimepiride, selectivity, precision, accuracy, and robustness. The LOD and LOQ were 0.315 and 1.050 mg/L, respectively. The multivariate strategy adopted in this work can be successfully applied in routine laboratories because of its fast optimization without the additional cost of columns or equipment.Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq