scholarly journals SIMULTANEOUS ESTIMATION OF LOPERAMIDE HYDROCHLORIDE AND TINIDAZOLE IN BULK AND FORMULATIONS BY REVERSE PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

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>

2019 ◽  
Vol 9 (4-s) ◽  
pp. 165-170
Author(s):  
Komal Gupta ◽  
Deepika Sharma ◽  
Pooja Chawla

Background: Racecadotril and Ofloxacin (RACIGYL- O) drug combination are used for the treatment of diarrhea. The drugs have been estimated individually in formulations but no method has been developed for simultaneous estimation of these two drugs as combination. Objective: To develop and validate a high performance liquid chromatography method for the simultaneous estimation of Racecadotril and Ofloxacin in tablet dosage form. Method: A WATERS C18 column (250 x 4.6mm, 5 μm) with mobile phase consisting of acetonitrile, methanol and water 40:40:20v/v (pH adjusted to 2.7 of water with ortho phosphoric acid). The flow rate was 1.0mL/min and effluents were monitored at 210nm. Results: The retention time of RAC and OFL was 4.666 min and 2.551 min respectively. The developed method was validated according to ICH guidelines with respect to specificity, linearity, accuracy, precision, robustness, Limit of Detection (LOD) and Limit of Quantification (LOQ). Conclusion: The method show good reproducibility and recovery with %RSD less than 2. So the proposed method was found to be simple, rapid, precise and accurate and useful for the determination of RAC and OFL in bulk and pharmaceutical dosage forms.   Keywords: RP-HPLC, Racecadotril, Ofloxacin, ICH guidelines.


Author(s):  
RASHMI PATIL ◽  
UTTARA JAISWAR ◽  
VANDANA JAIN

Objective: The study aims to develop and validate a novel reverse-phase high-performance liquid chromatographic method for simultaneous estimation of andrographolide and aloe-emodin in herbal formulation and validate as per the International Conference on Harmonization (ICH) guidelines. Methods: The analysis was carried on a Shimadzu LC Prominence-i 2030 model with the Lab Solution software. The column used for separation was Prontosil C18 (250×4.6 mm, 5 μ), with a mobile phase consisting of acetonitrile and 0.05% orthophosphoric acid (45:55), at a flow rate of 1 ml/min, column temperature was maintained at 28°C and effluents were monitored at 225 nm. The injection volume was 10 μl. Results: The retention time of andrographolide and aloe-emodin was found to be 4.57±0.2 min and 12.29±0.2 min, respectively. The markers were resolved using linear responses that were obtained in concentration ranges of 0.5–60 μg/ml with correlation coefficient (r2) of 0.9992 and 0.999 for andrographolide and aloe-emodin, respectively. The precision results were found to be satisfactory, which indicates that the method is precise. The recovery values lie in the range of 98–120% indicating the accuracy of the method. Conclusion: A novel, simple, accurate, precise, and robust reverse-phase high-performance liquid chromatography method was developed for the simultaneous estimation of andrographolide and aloe-emodin. The developed method can be used for analysis of the formulations containing these phytoconstituents.


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):  
MEGHA PATEL ◽  
PARESH PATEL ◽  
DHARA PATEL

Objective: A simple, rapid, accurate, precise, specific, and sensitive reverse-phase high-performance liquid chromatography (RP-HPLC) method has been developed and validated for simultaneous estimation of olanzapine (OLZ) and aripiprazole (APR) in synthetic mixtures. Methods: The stationary phase used for chromatographic separation was Phenomenex C18 column (250 mm × 4.6 mm i.d, particle size 5 μm) and mobile phase used for separation was methanol: Phosphate buffer (pH 3) taken in ratio of 75:25 %v/v. The flow rate was used 1.0 ml/min at room temperature and drugs detected at 240 nm with injection volume 20 μL. Results: The retention time for OLZ and APR was found to be 4.231 and 6.523 min, respectively. The linearity was performed using a concentration range of 0.5–3.0 for both drugs. The correlation coefficient was found to be 0.999 for OLZ and APR. The % purity of both the drug was found to be 98–102%. The proposed RP-HPLC method has been validated, according to International council on harmonization Q2 (B) guidelines. Conclusion: There was no interference of any diluents and excipients in the determination of drugs from synthetic mixture. Hence, the developed method can be used for routine quality control analysis.


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):  
Anjoo Kamboj ◽  
Manisha Bhatti ◽  
Pooja Atri

ABSTRACTObjective: Xanthium strumarium is a cocklebur or burweed belonging to family Asteraceae and commonly found as a weed, is widely distributed inNorth America, Brazil, China, Malasia, and hotter part of India. The herb is traditionally used mostly in treating several ailments. The present studydeals with development and validation of a reliable reverse phase high-performance liquid chromatography (RP-HPLC) method for the simultaneousestimation of Stigmasterol and β-sitosterol in the various extracts of the plant.Methods: The proposed method utilizes a Qualisil Gold C18 column (250×4.6 mm), 5 µm particle size, under isocratic elution conditions with themixture of acetonitrile:ethanol:water (85:14:1 v/v/v) at 25° as a mobile phase. An effluent flow rate of 1 ml/minute and ultraviolet detection at202 nm was used for the analysis of Stigmasterol and β-sitosterol.Results: The described method was linear in the range of range of 100-500 µg/ml and 10-500 µg/ml for stigmasterol and β-sitosterol respectively,with excellent correlation coefficients. The precision, robustness, and ruggedness values were also within the prescribed limits (<2%). The recoveryvalues were within the range, which indicates that the accuracy of the analysis was good and that the interference of the matrix with the recovery ofphytosterols was low. The phytosterols were found to be stable in a stock solution for 24 hrs (percentage relative standard deviation was below 2%)and no interfering extra peaks were observed under controlled stress conditions.Conclusion: The proposed method is simple, specific, precise, accurate, and reproducible and thus can be used as appropriate method for routineanalysis of X. strumarium phytosterols in quality control laboratories.Keywords: Xanthium strumarium, Reverse phase high-performance liquid chromatography method, Precision, Phytosterols, Quality control.


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