Development and validation of analytical methods for characterization and quantifi...
| Grant number: | 11/03307-4 |
| Support type: | Scholarships in Brazil - Master |
| Effective date (Start): | August 01, 2011 |
| Effective date (End): | February 28, 2013 |
| Field of knowledge: | Health Sciences - Pharmacy - Medicines Analysis and Control |
| Principal Investigator: | Hérida Regina Nunes Salgado |
| Grantee: | Tahisa Marcela Pedroso |
| Home Institution: | Faculdade de Ciências Farmacêuticas (FCFAR). Universidade Estadual Paulista (UNESP). Campus de Araraquara. Araraquara , SP, Brazil |
Abstract The antimicrobials have a crucial role in the control of infectious diseases. Cephalosporins remain one class of antimicrobials that stand out for their therapeutic importance, high frequency of use, safety and effectiveness against a broad microbial spectrum. Cefazolin sodium (CFZ) is a ²-lactam antimicrobial agent, classified as first-generation cephalosporin, often used as a therapeutic agent and for perioperative prophylaxis. In this work, new analytical methods were developed for qualitative and quantitative analysis of cefazolin sodium in lyophilized powder, seeking obtain method faster, safer for operators, more economical and easiness of implementation, which are essential for the analysis of this cephalosporin in pharmaceutical industry. For qualitative analysis, several methods were performed, including analyzes of solubility, melting point and pH; ultraviolet (UV) and infrared (IR) spectrophotometry; thin layer chromatography and high performance liquid chromatography (HPLC) allowing the identification of samples. For quantification of the drug, three analytical methods were validated. The spectrophotometric method in the ultraviolet region was validated at 270 nm, with a linear range of concentration from 8 to 28 mg/mL, using purified water as solvent, the content of 99.10% accuracy of 100.56%. In the microbiological assay by turbidimetric method, Staphylococcus aureus ATCC 26923 was used as microrganism test, with linear range from 6 to 11.46 mg/mL, the method presented potency of 100.07% and accuracy of 99,92%. Validation of the HPLC method consisted of mobile phase composed of purified water and acetonitrile (60:40 v/v), adjusted to pH 8 with triethylamine (TEA), and detection wavelength of 270 nm, yielding a retention time of 3.6 minutes in the linear range evaluated from 30 to 80 µg/mL, content of 100.39% accuracy of 100.37%. The developed methods showed excellent validation results, and the statistical analysis corroborated for its assessment. The developed methods showed no statistical difference for a significance level of 5%, proving to be equivalent to the quantification of cefazolin sodium in samples of lyophilized powder for injectable solution. The methods developed have met all requirements demanded by official agencies BRAZILIAN PHARMACOPEIA, FDA and ICH, shown to be appropriate and simple, could be used for the analysis of cefazolin sodium powder lyophilized for injectable solution in the pharmaceutical industry, helping to improve the quality control of the drug marketed. (AU) | |