Validated method for the determination of Gemifloxacin in bulk, pharmaceutical formulations and human serum by RP-HPLC: in vitro applications

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.

Monitoring of Pregabalin in Pharmaceutical Formulations and Human Serum Using UV and RP-HPLC Techniques: Application to Dissolution Test Method

“…These all were quite exclusive methods because of their extended and monotonous pretreatment of the samples, extraction with solvent and derivatization for the analysis of pregabalin. Our research group has reported a number of LC methods for the determination of various drugs as quinolones [13][14][15], cephalosporines [16], Ca channel blockers [17], ACE inhibitors [18][19][20][21] and antidiabetic drugs [22][23][24][25][26][27]. In continuation with this work we report are rapid, sensitive, selective, precise, short time analysis and cost effective RP-HPLC method for the quantitation of pragabalin in API, dosage formulations and human serum, the method is being validated according to ICH guidelines [28,29].…”

Facile LC‐UV methods for simultaneous monitoring of ciprofloxacin and rosuvastatin in API, formulations and human serum

“…Many analytical methods have been developed to determine statins, specifically rosuvastatin alone, such as liquid chromatography (Pasha et al ., ), or in combination with other drugs over the past decade as with simvastatin and pravastatin sodium (Chaudhari et al ., ), atorvastatin, lovastatin, pravastatin and simvastatin (Pasha et al ., ), with finofibrate (Sharma and Bhandari, ), with atenolol, spironolactone, glibenclamide and naproxen sodium (Sultana et al ., ), with pioglitazone, gliquidone and simvastatin, with simvastatin, atorvastatin, pravastatin and ceftriaxone (Arayne et al ., ), with diltiazem, atorvastatin and simvastatin (Sultana et al ., ), with lisinopril, pravastatin and atorvastatin (Sultana et al ., ), with captopril, atorvastatin and simvastatin (Sultana et al ., ), with Angiotensin Converting Enzyme (ACE) inhibitors (Arayne et al ., ) and with Non Steroidal Antiinflammatory Drugs (NSAIDs) (Arayne et al ., ; Sultana et al ., ). A number of spectrophotometric and RP‐HPLC methods have been reported for the quantitative determination of fluoroquinolones in pharmaceutical formulations and spiked human serum (Joshi, ; Belal et al ., ; Santoro et al ., ; Arayne et al ., ; Sultana et al ., ) as well as simultaneous determination of quinolones with other co‐administered drugs (Gul et al ., ; Sultana et al ., ,,, ).…”

High Throughput Quantitative Bioanalytical LC/MS/MS Determination of Gemifloxacin in Human Urine

“…An extensive literature survey revealed that several analytical methods have been reported for the determination of gemifloxacin in pharmaceutical preparations or human plasma or even in honey. Such methods are the various spectrophotometric techniques [16][17][18][19][20][21][22][23][24][25], capillary electrophoresis [26], high performance liquid chromatography [27][28][29][30][31][32][33][34][35][36], LC-mass spectrometry [37][38][39][40][41], microchip electrophoresis [42], chemiluminescence [43] and potentiometry [44] These methods were related to some major drawbacks such as having inadequate sensitivity, being time-consuming, tedious and sophisticated sample preparation. However, to the best of our knowledge, determination of GFX with complete validation in human urine has never been published.…”