Fotodegradação de esparfloxacino e isolamento de seus produtos de degradação utilizando CLAE

Sparfloxacin, a third generation fluoroquinolone derivative,is a potent antibacterial agent active against a wide range ofGram-positive and Gram-negative organisms including Streptococcus pneumoniae, Staphylococcus aureus, methicillinresistant S. aureus, Legionella spp., Mycoplasma spp.,Chlamydia spp. and Mycobacterium spp. A drawback offluoroquinolones is their photoreactivity. Sparfloxacin hasbeen studied in terms of therapeutic activities. However, the reare few published of analytical methods being applied tosparfloxacin. The aim in this study was to determine the photodegradation products of sparfloxacin, when submittedto UV light, and to characterize two of these products,designated SPAX-PDP1 and SPAX-PDP2. An acceleratedstudy of stability in methanol solution was carried out byexposing a solution of sparfloxacin to UV light (peakwavelength 290 nm) for 36 hours at room temperature. Theproducts were analyzed by NMR spectrophotometry, IR spectrometry and mass spectrophotometry. The result ssuggest that the products isolated here could be used toestimate the degradation of sparfloxacin in a stability study. However, the low activity exhibited by UV-irradiated sparfloxacin is a source of concern that demands further investigation of the mechanism of its photodegradation mechanism.Esparfloxacino, fluorquinolona de terceira geração, é umpotente agente antibacteriano ativo contra Gram-positivos eGram-negativos, incluindo Streptococcus pneumoniae,Staphylococcus aureus, S. aureus meticilina resistentes,Legionella spp., Mycoplasma spp., Chlamydia spp. eMycobacterium spp. Um aspecto importante dasfluorquinolonas é sua fotoinstabilidade. O esparfloxacino temsido amplamente estudado em termos de atividadesterapêuticas. Entretanto, poucos relatos a respeito de métodosanalíticos para esta quinolona são disponíveis na literatura. O objetivo deste trabalho foi determinar a fotoestabilidadede esparfloxacino submetido à luz UV, bem como caracterizar dois produtos, codificados como SPAX-PDP1 e SPAX-PDP2. Um estudo acelerado de estabilidade foi realizado submetendo-se o esparfloxacino a luz UV (comprimento de onda 290 nm) durante 36 horas em temperatura ambiente. Os resultados foram analisados por espectrofotômetro de massas, de RMN de 1H e de 13C e espectrometria na região de infravermelho. Os resultados sugerem que os produtos isolados podem ser usados para determinar a degradação de esparfloxacino em estudos de fotoestabilidade. No entanto, abaixa atividade do esparfloxacino submetido à luz UV demonstra a necessidade de investigações a respeito do mecanismo de fotodegradação deste fármaco

Byrsonima Crassa Niedenzu (ik): Antimicrobial Activity And Chemical Study

The methanolic extract of leaves from Byrsonima crassa, a Brazilian medicinal plant, was analyzed by CC and HPLC. Four constituents were isolated and identified as quercetin, methyl gallate, (-)-epigallocatechin gallate and quercetin-3-O-(2″-galloyl)-α-L-arabinopyranoside. The methanolic and hydromethanolic extract, as well as fractions, were evaluated regarding their possible antimicrobial activity using in vitro methods. Results showed that both extracts and fractions exhibited significant antimicrobial activity against all tested strains.2617175Agrawal, P.K., (1989) Carbon 13NMR of Flavonoids, , Amsterdam:ElsevierAlzoreky, N.S., Nakahara, K., Antibacterial activity of extracts from some edible plants commonly consumed in Asia (2003) Int J Food Microbiol, 80, pp. 223-230Amarqiuise, A., Che, C.T., Bejar, E., Malone, M.H., Fong, H.H.S., A New Glycolipid from Byrsonima crassifolia (1994) Planta Med, 60, pp. 85-86Basile, A., Sorbo, S., Giordano, S., Ricciardi, L., Ferrara, S., Montesano, D., Cobianchi, R.C., Ferrara, L., Antibacterial and allelopathic activity of extract from Castanea sativa leaves (2000) Fitoterapia, 71, pp. S110-S116Bauer, A.W., Kirby, M.D.K., Sherries, J.C., Truck, M., Antibiotic susceptibilities testing by standard single disc diffusion method (1966) Am J Clin Pathol, 45, pp. 493-496Bejar, E., Amarquaye, A., Che, C.T., Malone, M.H., Fong, H.H.S., Constituents of Byrsonima crassifolia and their spasmogenic activity (1995) Int J Pharmacog, 33, pp. 25-32Binutu, O.A., Cordell, G.A., Gallic acid derivatives from Mezoneuron benthamianum leaves (2000) Pharm Biol, 38, pp. 284-286Djipa, C.D., Delmee, M., Quetin-Leclercq, J., Antimicrobial activity of bark extracts of Syzygium jambos (L.) Alston (Myrtaceae) (2000) J Ethnopharmacol, 71, pp. 307-313Geiss, F., Heinrich, M., Hunkler, D., Rimpler, H., Heinrich, M., Proanthocyanidins with (+)-epicatechin units from Byrsonima crassifolia bark (1995) Phytochemistry, 39, pp. 635-643Gottlieb, O.R., Henriques Mendes, P., Taveira Magalhães, M., Triterpenoids from Byrsonima verbascifolia (1975) Phytochemistry, 14, pp. 1456-1456Harborne, J.B., (1996) The Flavonoids: Advances in Research since 1986, , New York:Chapman & HallLopez, A., Hudson, J.B., Towers, G.H.N., Antiviral and antimicrobial activities of Colombian medicinal plants (2001) J Ethnopharmacol, 77, pp. 189-196Martínez-Vasquéz, M., González-Esquinca, A.R., Cazares Luna, L., Moreno Gutiérrez, M.N., García-Argáez, A.N., Antimicrobial activity of Byrsonima crassifolia (L.) H.B.K (1999) J Ethnopharmacol, 66, pp. 79-82Mendes, C.C., Cruz, F.G., David, J.M., Nascimento, I.P., David, J.P., Triterpenes esterified with fatty acid and triterpene acids isolated from Byrsonima microphylla (1999) Quím Nova, 22, pp. 185-188Nascimento, G.G.F., Locatelli, J., Freitas, P.C., Silva, G.L., Antibacterial activity of plants extracts and phytochemicals on antibiotic-resistant bacteria (2000) Braz J Microbiol, 31, pp. 247-256(2003) Performance Standards for Antimicrobial Disc Susceptibility Tests, , Approved Standard M2-A7, Pennsylvania:WaynePenna, C., Marino, S., Vivot, E., Cruanes, M.C., Munoz, J.D., Cruanes, J., Ferraro, G., Martino, V., Antimicrobial activity of Argentine plants used in the treatment of infectious diseases. Isolation of active compounds from Sebastiania brasiliensis (2001) J Ethnopharmacol, 77, pp. 37-40Pretorius, J.C., Magama, S., Zietsman, P.C., Purification and identification of antibacterial compounds from Euclea crispa subsp crispa (Ebenaceae) leaves (2003) S Afr J Bot, 69, pp. 579-586Rastrelli, L., De Tommasi, N., Berger, I., Caceres, A., Saravia, A., De Simone, F., Glycolipids from Byrsonima crassifolia (1997) Phytochemistry, 45, pp. 647-650Sannomiya, M., Rodrigues, C.M., Coelho, R.G., Santos, L.C., Hiruma-Lima, C.A., Souza Brito, A.R.M., Vilegas, W., Application of preparative high-speed counter-current chromatography for the separation of flavonoids from the leaves of Byrsonima crassa Niedenzu (IK) (2004) J Chromatogr A, 1035, pp. 47-51Sannomiya, M., Fonseca, V.B., Da Silva, M.A., Rocha, L.R.M., Dos Santos, L.C., Souza, H.C.A., Brito, A.R.M., Vilegas, W., Flavonoids and antiulcerogenic activity from Byrsonima crassa leaves extracts (2005) J Ethnopharmacol, 97, pp. 1-6Silva, S.R., Silva, A.P., Munhoz, C.B., Silva Jr., M.C., Medeiros, M.B., (2001) Guia de Plantas Do Cerrado Utilizadas Na Chapada Dos Veadeiros, , Brasília:WWF58pSrinivasan, D., Nathan, S., Suresh, T., Perumalsamy, P.L., Antimicrobial activity of certain Indian medicinal plants used in folkloric medicine (2001) J Ethnopharmacol, 74, pp. 217-220Wagner, H., Bladt, H., Zgainski, E.M., (1984) Plant Drug Analysis, , Berlin:Springer320

Thermal analysis of sparfloxacin

Foi realizada a análise térmica de esparfloxacino,fluorquinolona de terceira geração que possui potenteatividade contra bactérias Gram-positivas, como Streptococcus pneumoniae e Staphylococcus aureus inclusive cepas meticilina resistentes (MRSA), bactériasGram-negativas, anaeróbios, Legionella spp., Mycoplasma spp., Chlamydia spp. e Mycobacterium spp. Nas curvas DTA observa-se pico endotérmico de fusãona temperatura de 276,5 °C. A curva DTA, em ar sintético,apresenta dois picos exotérmicos (341,6 e 579,2 °C), atribuídos à decomposição do composto. A curva TG permite observar a perda de massa total em duas etapas,entre as temperaturas 285,5 e 645,3 °C. A curva DTA,em atmosfera de nitrogênio, apresenta pico exotérmicode decomposição na temperatura de 340,0 oC e na curva TG, a perda de massa inicia-se na temperatura de 254,4 °C.Sparfloxacin, a third-generation fluoroquinolone, is a potent antibacterial agent against a wide range of Grampositive and Gram-negative organisms, for example Streptococcus pneumoniae, Staphylococcus aureus (including methicillin-resistant strains), Legionella spp., Mycoplasma spp., Chlamydia spp. and Mycobacterium spp. This compound has been submitted to thermal analysis and the results are presented here. The DSC curve of sparfloxacin has an endothermic peak that indicates a melting point at 276.5 °C. The DTA curve of the sample in synthetic air shows two exothermic peaks, at 341.6 and 579.2 °C, attributed to compound decomposition. In the TG curve, the loss of mass can be seen to occur in two steps between 285.5 and 645.3 °C. The DTA curve obtained in a nitrogen atmosphere shows an exothermic peak, with decomposition of sparfloxacin at 340.0 °C; from the corresponding TG plot, the loss of mass starts at 254.4 °C

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 <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

Antimicrobial activity of Davilla elliptica St. Hill (Dilleniaceae)

Davilla elliptica St. Hill ("lixinha"), family Dilleniaceae, is commonly used in the Brazilian folk medicine as purgative and stimulant. This work evaluated the antimicrobial activity of the methanol and chloroform extracts of the leaves and barks of D. elliptica using the disc-diffusion method. The results obtained showed that the methanolic extracts of the leaves and barks presented antimicrobial activity against the tested microorganisms