High-performance liquid chromatography thermodynamic study of new potential antiepileptic compounds on a cholesterol column using isocratic elution with methanol/water and acetonitrile/water eluent systems

2017 ◽  
Vol 40 (21) ◽  
pp. 4176-4190 ◽  
Author(s):  
Jolanta Flieger ◽  
Hanna Trębacz ◽  
Magdalena Pizoń ◽  
Anna Kowalska ◽  
Agnieszka Szczęsna ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Thermodynamic Study ◽  
Isocratic Elution

Analysis of organic impurities of besifloxacin hydrochloride by high performance liquid chromatography with isocratic and gradient elution.

2019 ◽  
Vol 16 ◽  
Author(s):  
Joanna Wittckind Manoel ◽  
Camila Ferrazza Alves Giordani ◽  
Livia Maronesi Bueno ◽  
Sarah Chagas Campanharo ◽  
Elfrides Eva Sherman Schapoval ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Gradient Elution ◽  
Pharmaceutical Product ◽  
Raw Material ◽  
Isocratic Elution ◽  
Organic Impurities ◽  
Elution Method

Introduction: Impurity analysis is an important step in the quality control of pharmaceutical ingredients and final product. Impurities can arise from drug synthesis or excipients and even at small concentrations may affect product efficacy and safety. In this work two methods using high performance liquid chromatography (HPLC) were developed and validated for the evaluation of besifloxacin and its impurity synthesis, with isocratic elution and another with gradient elution. Method: The analysis by HPLC in isocratic elution mode was performed using a cyano column maintained at 25 °C. The mobile phase was composed by 0.5% triethylamine (pH 3.0): acetonitrile (88:12 v/v) eluted at a flow rate of 1.0 ml/min with detection at 330 nm. The gradient elution method was carried out with the same column and mobile phase components only modifying the rate between organic and aqueous phase during analysis. The procedures have been validated according to internationally accepted guidelines, observing results within acceptable limits. Results: The methods presented were found to be linear in the 140 to 260 µg/ml range for besifloxacin and 0.3 to 2.3 µg/ml for an impurity named A. The limits of detection and quantification were respectively 0.07 and 0.3 µg/ml for impurity A, with a 20 µL injection volume. The precision achieved for all analyses performed provided RSD inter-day equal to 6.47 and 6.36% for impurity A with isocratic elution and gradient, respectively. The accuracy was higher than 99% and robustness exhibited satisfactory results. In the isocratic method an analysis time of 25 min and 15 min was obtained for gradient. For impurity A, the number of theoretical plates in the isocratic mode was about 5000 while in the gradient mode it was about 45000, hence, it made the column more efficient by changing the mobile phase composition during elution. In besifloxacin raw material and in pharmaceutical product used in this study, other related impurities were present but but impurity A was searched for and not detected Conclusion: The proposed methods can be applied for quantitative determination of impurities in the analysis of the besifloxacin raw material, as well as in ophthalmic suspension of the drug, considering the quantitation limit.

scholarly journals Simultaneous Determination of Phenolic Compounds in Leptadenia pyrotechnica (Forssk.) Decne. by Using High-Performance Liquid Chromatography (HPLC-DAD-UV)

2018 ◽  
Vol 2018 ◽  
pp. 1-4
Author(s):  
Raman Preet ◽  
Raghbir Chand Gupta
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Phenolic Compounds ◽  
Mobile Phase ◽  
High Performance ◽  
Isocratic Elution ◽  
Methanolic Extracts ◽  
Aerial Parts ◽  
Whole Plant

During the present study, an endeavor has been made to produce a simple, rapid, and simultaneous method for determination of phenolic compounds by using high-performance liquid chromatography in aerial parts of Leptadenia pyrotechnica (Forssk.) Decne. collected from the Indian Thar Desert. The optimized process was used for the quantification of ten phenolic compounds. The chromatographic separation was accomplished on an Atlantis T3 column at 25°C with isocratic elution. A mixture of acetonitrile and water was used as the mobile phase at a flow rate of 0.8 mL/min. The linear regression examination data for the calibration plots displayed a good linear relationship with r2 > 0.999 in the concentration range of 2–20 µL. In the methanolic extracts of the whole plant of L. pyrotechnica, the content of caffeic acid (3.3%) was reported to be the highest concentration.

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