No abstract

Um método isocrático de cromatografia líquida de alta resolução de fase reversa (RP-HPLC) foi desenvolvido para determinação de gemifloxacin a granel, em formulações e soro humano a 270 nm. A separação cromatográfica foi adquirida em uma coluna Purospher STAR C 18 (250 × 4,6 mm, 5 µm) usando a fase móvel metanol:água (90:10, v/v) ajustada para pH 2,8 com ácido fosfórico 85% em fluxo de 1,5 mL min -1 a temperatura ambiente. As curvas de calibração mostraram-se lineares dentro do intervalo de 5-100 µg mL -1 com um coeficiente de correlação de 0,9998. Os limites de detecção (LOD) e de quantificação (LOQ) foram 0,015 and 0,045 µg mL -1 , respectivamente. Os resultados de precisão intra-e inter-corridas e de exatidão foram 98,73-100,12%, que foram correlacionados através do teste t student. Este método foi aplicado para interações in vitro do gemifloxacino com elementos essencial e traço.An isocratic reversed phase high-performance liquid chromatographic (RP-HPLC) method has been developed for the determination of gemifloxacin in bulk, dosage formulations and human serum at 270 nm. Chromatographic separation was achieved on Purospher STAR C 18 (250 × 4.6 mm, 5 µm) column using mobile phase methanol:water (90:10, v/v) adjusted pH 2.8 via phosphoric acid 85% having flow rate of 1.5 mL min -1 at ambient temperature. Calibration curves were linear over range of 5-100 µg mL -1 with a correlation coefficient 0.9998. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.015 and 0.045 µg mL -1 , respectively. Intra and inter-run precision and accuracy results were 98.73-100.12% and then correlated through student's t-test. This method was further applied for in vitro interactions of gemifloxacin with essential and trace elements.

A simple reversed phase HPLC method have been successfully developed and validated for the quantitative determination of moxifloxacin (MOX) in bulk material, pharmaceutical formulation and serum. Purospher STAR C18 (25 cm × 4.6 mm, 5 μm) and Discovery C18 (25 cm × 4.6 mm, 5 μm) columns were used. The mobile phase, methanol: acetonitrile: water (85:5:10, v/v/v), pH 2.75 adjusted by phosphoric acid was delivered at a flow rate of 1 mL min−1. The eluents was monitored using UV detector at 290 nm. The proposed method is specific, accurate (99.39‐102.67%), precise (intra‐day variation 0.04‐0.86% and inter‐day variation 0.12‐0.94%) and linearity (R2 > 0.999) within the desired range 0.39‐25 μg mL−1 concentration. The detection and quantification limit was 0.002‐0.51 μg mL−1 and 0.01‐0.555 μg mL−1, respectively. The analysis of variance (ANOVA) and student's t‐test were applied to verify the results. The anticipated method is applicable to routine analysis of MOX in pharmaceutical formulations and human serum samples. It is also applied on interaction of MOX with several essential and trace metals as well as interaction with antacids.

A simple reversed phase HPLC method was developed and validated for the simultaneous determination of sparfloxacin (SPFX), diclofenac sodium, meloxicam, ibuprofen, flurbiprofen, naproxen and mefenemic acid in a relatively short time with high linearity in bulk material, pharmaceutical formulations and human serum. Purospher STAR C 18 (250 × 4.6 mm, 5 μm) column was utilized with mobile phase, methanol and water (90:10, v/v pH 2.70 adjusted by phosphoric acid), was delivered at a flow rate of 1.5 mL·min -1 . Eluent was monitored using UV detector at 240 nm. The proposed method is specific, accurate (98.42% -102.75%), precise (intra-day and inter-day variation 0.011% -1.85%) and linear (R 2 > 0.999) with in the desired range 0.15 -40 µg·mL -1 and the detection and quantification limit was 1.19E+08 -0.150 µg·mL -1 and 3.62E+08 -0.4574 µg·mL -1 respectively for SPFX and NSAIDs. The analysis of variance (ANOVA) and student's t-test were applied to verify the results. The anticipated method is applicable to routine analysis of SPFX and NSAIDs in pharmaceutical formulations as well as in human serum samples. It has also applied on interaction of SPFX with NSAIDs.

Four new metal complexes (S12-S15) of SPFX (third-generation quinolones) via heavy metals have been synthesized in good yield and characterized by physicochemical and spectroscopic methods including TLC, IR, NMR, and elemental analyses. Sparfloxacinato ligand binds with metals through pyridone and oxygen atom of carboxylic group. The biological actives of complexes have been tested against four Gram-positive and seven Gram-negative bacteria and six different fungi. Statistical analysis of antimicrobial data was done by one-way ANOVA, Dunnett's test; it was observed that S13, S14, and S15 were found to be most active complexes. Antifungal data confirm that all four synthesized complexes are most active and show significant activity against F. solani with respect to parent drug and none of complexes show activity against A. parasiticus, A. effuris, and S. cervicis. To study inhibitory effects of newly formed complexes, enzyme inhibition studies have been conducted against urease,-chymotrypsin, and carbonic anhydrase. Enzymatic activity results of these complexes indicated them to be good inhibitors of urease enzyme while all complexes show mild activities against carbonic anhydrase enzyme. Further research may prove the promising role of these synthesized complexes as urease inhibitors.