scholarly journals DEVELOPMENT AND VALIDATION OF A STABILITY INDICATING REVERSE PHASEHIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR SIMULTANEOUS DETERMINATION OF CLINDAMYCIN, METRONIDAZOLE, AND CLOTRIMAZOLE IN PHARMACEUTICAL COMBINED DOSAGE FORMS

Author(s):  
Revathi Naga Lakshmi Ponnuri ◽  
Prahlad Pragallapati ◽  
Mastanamma Sk ◽  
Ravindra N ◽  
Venkata Basaveswara Rao Mandava ◽  
...  

ABSTRACTObjective: The objective of present work was to develop and validate a simple, fast, precise, selective, and accurate reverse phase high-performanceliquid chromatography method for the simultaneous determination of Clindamycine, Metronidazole and Clotrimazole in a pharmaceutical dosageform.Methods: The separation of these three drugs was achieved on ODS 250×4.6 mm, 5 mm C column. Mobile phase containing 0.1% ortho phosphoricacid buffer and acetonitrile in the ratio of 55:45 v/v was pumped through column at a flow rate of 1 ml/minute. Temperature was maintained at 30°Cand ultraviolet detection at 238 nm.18Results: The retention times were observed to be 2.591, 3.584, and 4.221 minutes for Clindamycine, Metronidazole, and Clotrimazole, respectively.Linearity was found to be 25-150 μg/ml Clindamycine, Metronidazole, and Clotrimazole, respectively. The method was statistically validated forlinearity, recovery, the limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision. The stress testing of the drugs individually andtheir mixture are carried out under acidic, alkaline, oxidation, photostability, and thermal degradation conditions and its degradation products arewell resolved from the analyte peaks.Conclusion: This method was successfully validated for accuracy, precision, and linearity, LOD, and LOQ.Keywords: Clindamycine, Metronidazole, Clotrimazole, Reverse phase-high performance liquid chromatography, Simultaneous determination,Degradation studies.

Author(s):  
BYRAN GOWRAMMA ◽  
SUBRAMANIYAN NAIYANAR MEYYANATHAN ◽  
BASAWAN BABU ◽  
NAGAPPAN KRISHNAVENI

Objective: In the present study, an isocratic chiral reverse-phase high-performance liquid chromatography method was developed and the resolution of the drug and complete separation from its degradation products were successfully achieved. Methods: An isocratic method developed with a Phenomenex Lux 5 μ Cellulose 1 (150 mm×4.6 mm i.d., 5 μ) using UV detector at wavelength of 220 nm, with a mobile phase consisting of methanol:0.1% diethylamine (60:40% v/v) and a flow rate of 1 ml/min. The drug was subjected to alkaline, acidic, neutral, oxidative, and photolytic to apply stress conditions. The stressed samples were analyzed by the proposed method. Results: The described method was linear over the range of 3–7 μg/ml for R-enantiomer and 9–21 μg/ml of S-enantiomer, respectively. The limit of detection and limit of quantification of R and S enantiomers were found to be 0.56 μg/ml and 0.18 μg/ml, respectively. Conclusion: The method provides good sensitivity and excellent precision and reproducibility. The developed method can be applied in the quality control of drug products.


Author(s):  
Poornima K. ◽  
Channabasavaraj Kp.

<p><strong>Objective: </strong>A new, rapid, selective, precise, accurate and economical, isocratic, reverse phase high-performance liquid chromatography method has been developed for simultaneous estimation of loperamide hydrochloride and tinidazole in bulk and in tablet formulations.</p><p><strong>Methods: </strong>The separation was achieved by using Lithosphere RP C-18, (250 x 4.6 mm, 5 µm) end capped column with a mobile phase containing sodium-1-octane sulfonate buffer: methanol: acetonitrile (40:30:30%v/v/v) pH adjusted to 4.0 (using dilute orthophosphoric acid). The flow rate was 1.0 ml/m and column effluent was monitored at 224 nm. The method was validated as per international conference on chemical harmonization (ICH) guidelines.</p><p><strong>Results</strong>:<strong> </strong>Tinidazole and loperamide hydrochloride were eluted at about 3.1 and 5.4 min respectively, indicating the shorter analysis time. The proposed method was found to be accurate, precise and reproducible. The linearity was established in the concentration range of 10-50 µg/ml. Limit of detection (LOD) and Limit of quantification (LOQ) was found to be 0.001 µg/ml and 0.003 µg/ml for loperamide hydrochloride and 0.01 µg/ml and 0.03 µg/ml for tinidazole.</p><p><strong>Conclusion: </strong>This method can be used for routine analysis of formulations containing any of the above drugs or combinations without any alteration in the chromatographic conditions.</p>


2013 ◽  
Vol 57 (1) ◽  
pp. 25-32 ◽  
Author(s):  
Anna Gajda ◽  
Andrzej Posyniak ◽  
Andrzej Bober ◽  
Tomasz Błądek ◽  
Jan Żmudzki

Summary A liquid chromatography method with UV detection for determination of oxytetracycline (OTC) in honey has been developed. The samples were extracted with the solution of oxalic acid. The clean-up procedure was performed by solid phase extraction (SPE) using polymeric Strata X and carboxylic acid cartridges. Chromatographic separation was carried out on the Luna C8 analytical column with mobile phase consisting of acetonitrile-0.02 M oxalic acid. The method has been successfully validated according to the requirements of the European Decision 2002/657/EC and this method is used in routine control of oxytetracycline in honey samples. The limit of detection (LOD) and limit of quantification (LOQ) of the presented method were 10 and 12.5 μg/kg, respectively. The developed method has also been verified in quantitative determination of oxytetracycline residues in honey after experimental treatment with this product in bee colonies.


2020 ◽  
Vol 103 (4) ◽  
pp. 1181-1189
Author(s):  
Xiaoyun Duan ◽  
Xiaofeng Liu ◽  
Yue Dong ◽  
Jing Yang ◽  
Jing Zhang ◽  
...  

Abstract Background Sulfonamides have been widely used in the prevention and clinical treatment of bacterial diseases in livestock and poultry. The use of sulfonamides increases the risk of veterinary drug residues in animal derived foods. The traditional reversed phase liquid chromatography methods for sulfonamides residues detection in animal derived foods have the problem of high consumption of organic solvents. Objective The aim of this study was to establish a green high-performance liquid chromatography method for the detection of sulfonamides residues in different animal-origin foods. Method The sample extraction solutions were purified by the Agela Cleanert PEP-2 cartridge and analyzed by the high-performance liquid chromatography method using ethanol as the green alternative solvent. Results The proposed method was validated in terms of linear range (20–1000 μg/kg), limit of detection (3.0–12.3 μg/kg), limit of quantitation (10–43 μg/kg), accuracy (80.7–101.3%), and repeatability and reproducibility (RSD &lt;5.9% and RSD &lt;8.5% respectively). Conclusions The proposed method is an environmentally friendly, sensitive and reliable high-performance liquid chromatography method for simultaneous determination of sulfonamide residues in animal-origin foods. Highlights In this work, we firstly developed a green high-performance liquid chromatography method for simultaneous determination of the residues of nine sulfonamides in milk and beef with ethanol as the green alternative solvent.


2018 ◽  
Vol 2018 ◽  
pp. 1-5 ◽  
Author(s):  
Ahmed Salem Sebaei ◽  
Ahmed M. Gomaa ◽  
A. A. El-Zwahry ◽  
E. A. Emara

Formaldehyde is one of the most dangerous chemical compounds affecting the human health; exposure to it from food may occur naturally or by intentional addition. In this study a high performance liquid chromatography method for determination of formaldehyde in dairy products was described. The dairy samples were reacted and extracted with a warmed organic solvent in the presence of derivatizing agent 2,4-dinitrophenylhydrazine (DNPH) and formaldehyde; the mixture was centrifuged and followed by diode array detection. The method is validated and gives average recovery of formaldehyde at the three different levels 0.1, 5.0, and 10.0 mg/kg varied between 89% and 96%. The method is linear from the limit of quantification 0.1 mg/kg up to 10 mg/kg levels. This method is intended for formaldehyde analyses in dairy products simply with stable derivatization, minimum residue loss, excellent recovery, and accurate results with a sensitive limit of detection 0.01 mg/kg. 90 dairy samples from milk, cheese, and yogurt were investigated from seven Egyptian governorates and all samples were free from formaldehyde.


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