Validation of an UV method for the determination of ciprofloxacin in cocrystals
Amanda Cosmo de Almeida, Universidade Estadual Paulista, Araraquara, Brasil
Patrícia Osório Ferreira, Universidade Estadual Paulista, Araraquara, Brasil
Ana Carolina Kogawa, Universidade Estadual Paulista, Araraquara, Brasil (ac_kogawa@yahoo.com.br)
Flávio Junior Caires, Universidade Estadual Paulista, Araraquara, Brasil
Ciprofloxacin (CIP), the drug chosen for this study, has low aqueous solubility, which limits its bioavailability.CIP is a broad spectrum antibiotic that is used against Gram-negative and positive bacteria, as well as other microorganisms. A way to improve the solubility of CIP is through the cocrystal formation, that can be defined as a multicomponent crystal composed of active pharmaceutical ingredients and coformers, in a defined stoichiometric ratio, joined by intermolecular interactions. This work validated a UV spectrophotometric method for the determination of CIP in cocrystals, since in the literature have been reported many papers that determine ciprofloxacin hydrochloride. A stock solution containing 100 μg mL-1 of CIP was prepared with a 0.1 M HCl solution, using the ultrasound. Aliquots of the stock solution of ciprofloxacin were transferred to 10 mL volumetric flasks and the volume was then quenched with water. The readings were performed at a maximum wavelength of 277 nm using water as blank. This method showed linear regression in the concentration range of 2.0 to 7.0 µg mL-1. The linear equation was: y = 0.1282x + 0.0056, with a correlation coefficient equal to 0.9999.The RSD was 0.14%, 0.42% and 0.46% for the intra-day, inter-day and inter-analyst precision, respectively. This method proved to be accurate since the RSD were all less than 1%. The experimental concentrations that were found were very close to the theoretical concentrations, and the recoveries were between 98% and 102%. The method was robust in relation to the changes (the absence of filtration of the stock solution, the change of the wavelength to 275 nm and the use of a solution of HCl 0.08 M), because it presented low RSD values, all lower than 1.5%. The selectivity was verified by comparing the spectra obtained for the 4.0 μg mL-1 solutions of pure ciprofloxacin, diluent, coformers and cocrystals, and then the recovery values were calculated. The cocrystals used were CIP-INCA (30 Hz 90 min) and CIP-NCA/ EtOH (30 Hz). The selectivity shows that there was no interference on the part of the coformer or diluent for the cocrystals synthesized with isonicotinic (INCA) and nicotinic (NCA) acids. The CIP recovery for this cocrystals were 101.23% and 99.09%, respectively. So, the developed UV method was validated and was found to be accurate, precise, specific, linear and robust. No interference from coformers were observed.
Abstract Reference & Short Personal Biography of Presenting Author
So far, I have more than 60 scientific articles published. During my Master, PhD and post-doctoral studies I participated in national and international events through presentation of poster and oral papers in London (UK), Osaka (Japan), Valencia (Spain), Rome (Italy), Lisbon (Portugal), Berlin (Germany), Paris (France), Ghent and Liege (Belgium), Cordoba and Rosario (Argentina), Cartagena de las Indias (Colombia) and several cities in Brazil. I am a reviewer of 22 international journals, which are described in the curriculum. I co-supervised and co-supervise undergraduate, master and doctoral students. My index h = 10 and Index i10 = 10.
My area of activity is the physico-chemical and microbiological quality control of drugs and medicines aimed at green analytical chemistry and everything that involves it. Our concern for quality is multidimensional. It covers the health of the analyst, the chosen reagents, the treatment of residues, the amount of residues formed, the toxicity of the reagents, the accessories used, the analysis time, the chosen technique, the equipment of protection, physical and emotional well-being, the environment and, of course, safe and effective pharmaceutical analyzes.
My projects also aim to work in a multidisciplinary way interacting in different laboratories: Quality Control and Pharmaceutical Technology; different equipment: spectrophotometer, chromatograph, dissolutor, X-ray diffractor; different methods: wet milling, complexation, spectrophotometry in the ultraviolet, visible and infrared regions, high performance liquid chromatography, microbiological turbidimetry, dissolution; and different people. I believe that this interaction is rich and my goal is always to strengthen the group with the teachings brought and lived in other laboratories with other ways of working, I believe that networking nowadays is differential and can bring great opportunities. In this way, we improve ourselves, become integrated people and contribute to world literature and benefit the community, the population, since we think in a multidimensional way focusing on the whole, the parts and, above all, the interaction between the parts of a system.
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