scholarly journals Development and Validation of a Simple HPLC-UV Method for Determination of Amoxicillin trihydrate in Bulk Drug and Pharmaceutical Dosage Forms

2021 ◽  
Vol 4 (1) ◽  
pp. 72-83
Author(s):  
Tite Uwambajineza ◽  
Thomas Bizimana
Keyword(s):  
Organic Solvent ◽  
Mobile Phase ◽  
Environmentally Friendly ◽  
Dosage Forms ◽  
Test Method ◽  
Pharmaceutical Dosage Forms ◽  
Percent Recovery ◽  
Amoxicillin Trihydrate ◽  
Bulk Drug ◽  
Development And Validation

Background Many analytical methods for testing amoxicillin trihydrate from different monographs such as United States and British pharmacopoeia, use acetonitrile HPLC grade as an organic solvent in the mobile phase; however, this solvent is expensive and not environmentally friendly Objectives Developing and validating a simple, affordable, accurate, precise and environmentally friendly HPLC-UV method, for determining amoxicillin in formulations by using methanol HPLC grade as an organic solvent in the mobile phase Methods An HPLC system was used for developing and validation of laboratory test method which is less expensive and uses environmentally-friendly mixture of mobile phase solutions. Specificity, linearity, precision, repeatability, and accuracy were studied. Results The retention time (RT) for amoxicillin was 3.53 ± 0.020 min, and no interfering peaks were recorded with the blank, standard and sample at RT, ensuring specificity. Calibration curve of 20 to 160μg/ml was used. The correlation coefficient (r2) =0.9998, which indicates that the method has   the linearity to this range of 20 to 160μg/ml. Intra- and between days' repeatability were assessed by injecting solutions three times a day and within three days. The %RSD of 0.3% and 0.7% within and between days respectively, were recorded. The %RSD was ≤ 2%, which indicates a precision of the method. An average percent recovery of 100.5±3.6% was recorded. Conclusion An environmentally-friendly, simple, affordable, selective, specific, rapid, sensitive, repeatable, with precision and accurate HPLC-UV method, has been developed and validated for the estimation of amoxicillin trihydrate in pharmaceutical dosage forms and can be adopted for the purpose of quality control. Rwanda J Med Health Sci 2021;4(1):72-83

scholarly journals Validated RP-HPLC Method for the Determination of Ivabradine Hydrochloride in Pharmaceutical Formulation

2017 ◽  
Vol 9 (05) ◽  
Author(s):  
MD. Muzaffar -ur- Rehman1 ◽  
G. Nagamallika
Keyword(s):  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Bulk Drug

A simple, rapid, precise, and accurate RP-HPLC method for the estimation of Ivabradine Hydrochloride an anti-anginal agent, both as a bulk drug and in pharmaceutical formulation was developed. The chromatographic separation was achieved on a Thermosil C18 150 × 4.5 mm, 5μm column by using a mobile phase containing a mixture of methanol and phosphate buffer pH 6.5 in the ratio of 65:35 % v/v at a flow rate of 1ml/min and at an ambient temperature. The detection was monitored at a wavelength of 265nm. A clear chromatographic peak was identified with the retention time of 4.36 min and tailing factor of 1.23. The developed method was validated according to ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The method shows a good linear relationship with correlation co-efficient of more than 0.992 in the concentration range of 30μg-150μg. The method showed mean % Recovery of 100.4% and %RSD for repeatability and intermediate precision was less than 2%. The proposed method can be used successfully for the quantitative determination of Ivabradine HCL in pharmaceutical dosage forms.

scholarly journals QbD Approach for the Development and Validation of RP-UHPLC Method for Quantitation of Vildagliptin

2017 ◽  
Vol 16 (1) ◽  
pp. 107-117
Author(s):  
Sharifa Sultana ◽  
Uttom Kumar ◽  
Md Shahadat Hossain ◽  
Dilshad Noor Lira ◽  
Abu Shara Shamsur Rouf
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Quality By Design ◽  
Response Surfaces ◽  
Routine Analysis ◽  
Pharmaceutical Dosage Forms ◽  
Independent Variables ◽  
Two Factors ◽  
Bulk Drug ◽  
Development And Validation

The present work describes a quality by design (QbD)-based rapid, simple, precise and robust RPUHPLC method for the routine analysis of vildagliptin in bulk drug and in pharmaceutical dosage forms. Chromatographic separation was achieved by a X-bridge C18 column with isocratic elution of mobile phase containing mixture of phosphate buffer (pH 6.8) and acetonitrile in the ratio of 67:33(v/v). The flow rate was 1.0 ml/min and the detection was done at 239 nm with photo-diode array plus (PDA+) detector. The optimization of chromatographic method was carried out by QbD approach using design of experiments (DoE). Two factors utilized for the experimental design of the method were (i) independent variables which comprise percentages of acetonitrile in mobile phase and flow rate and (ii) co-variates which include the retention time, tailing factor and theoretical plates. This design was statistically analyzed by ANOVA, normal plot of residual, box-cox plot for power transform, perturbation, counter plot and 3D response surfaces plots. This was further validated as per the requirements of ICHQ2B guidelines for linearity, LOD, LOQ, accuracy, precision, specificity and robustness. The results showed that proposed method is simple, sensitive and highly robust for routine analysis of vildagliptin.Dhaka Univ. J. Pharm. Sci. 16(1): 107-117, 2017 (June)

scholarly journals RP-HPLC Analytical Method Development and Validation for Simultaneous Estimation of Three Drugs: Glimepiride, Pioglitazone, and Metformin and Its Pharmaceutical Dosage Forms

2013 ◽  
Vol 2013 ◽  
pp. 1-8 ◽  
Author(s):  
Gadapa Nirupa ◽  
Upendra M. Tripathi
Keyword(s):  
Analytical Method ◽  
Method Development ◽  
Dosage Forms ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Method Development And Validation ◽  
Bulk Drug ◽  
Development And Validation

Developing a single analytical method for estimation of individual drug from a multidrug composition is a very challenging task. A simple, rapid, precise, and reliable reverse phase HPLC method was developed for the separation and estimation of three drugs glimepiride, pioglitazone and metformin in bulk drug mix and pharmaceutical dosage forms. The estimation was carried out using Inertsil ODS-3V (250 mm × 4.6 mm, 5 μm) column; mobile phase consisting of acetonitrile, tetrahydrofuran, and buffer at pH 5; the flow rate of 1.7 mL/min and ultraviolet detection at 228 nm. All the three drugs were properly resolved having run time of 5 minutes, 3.9 minutes and 1.3 minutes for glimepiride, pioglitazone, and metformin, respectively. The method was validated as a final verification of method development with respect to precision, linearity, accuracy, ruggedness, and robustness. The validated method was successfully applied to the commercially available pharmaceutical dosage form, yielding very good and reproducible result.

scholarly journals Development and Validation of an HPLC Method for Determination of Ziprasidone and Its Impurities in Pharmaceutical Dosage Forms

2011 ◽  
Vol 94 (3) ◽  
pp. 713-722 ◽  
Author(s):  
Marija Pavlovic ◽  
Marija Malesevic ◽  
Katarina Nikolic ◽  
Danica Agbaba
Keyword(s):  
Mobile Phase ◽  
Raw Materials ◽  
Dosage Forms ◽  
Hplc Method ◽  
Array Detector ◽  
Least Squares Regression ◽  
Experimental Conditions ◽  
Pharmaceutical Dosage Forms ◽  
Development And Validation

Abstract Ziprasidone is known as a novel “atypical” or “second-generation” antipsychotic drug. A sensitive and reproducible method was developed and validated for determination of ziprasidone and its major impurities, which are significantly different in polarity. The separation is performed on a Waters Spherisorb® octadecylsilyl 1 column (5.0 μm particle size, 250 × 4.6 mm id) using a gradient with mobile phase A [buffer–acetonitrile (80 + 20, v/v)] and mobile phase B [buffer–acetonitrile (10 + 90, v/v)] at a working temperature of 25°C. The buffer was 0.05 M KH2PO4 solution with an addition of 10 mL triethylamine/L solution, adjusted to pH 2.5 with orthophosphoric acid. The flow rate was 1.5 mL/min, and the eluate was monitored at 250 nm using a diode array detector. Optimization of the experimental conditions was performed using partial least squares regression, for which four factors were selected for optimization: buffer concentration, buffer pH, triethylamine concentration, and temperature. The proposed validated method is convenient and reliable for the assay and purity control in both raw materials and dosage forms.

scholarly journals TLC-densitometric analysis of α-escin in bulk drug substance and in pharmaceutical dosage forms

2015 ◽  
Vol 28 (3) ◽  
pp. 186-191
Author(s):  
Malgorzata Dolowy ◽  
Alina Pyka-Pajak ◽  
Katarzyna Filip ◽  
Joanna Zagrodzka
Keyword(s):  
Sulphuric Acid ◽  
Mobile Phase ◽  
Stationary Phases ◽  
Dosage Forms ◽  
Oral Dosage ◽  
Pharmaceutical Dosage Forms ◽  
Drug Substances ◽  
Subsequent Application ◽  
Bulk Drug

Abstract A quite simple and rapid TLC-densitometric method for the identification of α-escin (Aescin) in bulk drug substances was developed. In so doing, different chromatographic conditions, including various mobile and stationary phases, were tested. A TLC densitometric determination of the examined compound was performed without using visualizing reagent, yet with the use of appropriate dipping reagents, in order to obtain reliable UV-densitometric measurements of α-escin - a substance which has weak chromophore groups. Herein, the application of a mobile phase containing n-butanolacetic acid-water in volume composition 30:7:13, the use of silica gel 60F254 plates with concentrating zone, and subsequent application of 10% sulphuric acid in ethanol or 5% vanillin in methanol/sulphuric acid, respectively, provided the best results in a TLCdensitometric study of α-escin. The described method was successfully employed to identify α-escin in commercial samples that were in an oral dosage form (tablets) and also in the form of gel containing 20 mg of α-escin.

Validated chiral chromatographic methods for clopidogrel bisulphate and its related substances in bulk drug and pharmaceutical dosage forms

2015 ◽  
Vol 69 (12) ◽  
Author(s):  
Eman S. Elzanfaly ◽  
Hala E. Zaazaa ◽  
Aya T. Soudi ◽  
Maissa Y. Salem
Keyword(s):  
United States ◽  
Thin Layer ◽  
Silica Gel ◽  
Mobile Phase ◽  
The United States ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Chromatographic Methods ◽  
Related Substances ◽  
Bulk Drug

AbstractTwo validated chromatographic methods developed for the analysis of S clopidogrel bisulphate in the presence of its related substances listed in the United States and British Pharmacopoeias including its inactive R enantiomer are described. The first method is a simple thin layer chromatographic (TLC) method where separation is performed on pre-coated silica gel 60 F254 plates using methanol/diethylamine/heptanes/water containing 20 mg vancomycin hydrochloride (7 : 7 : 1.5 : 0.5 vol. %) as a mobile phase. R

DETERMINATION OF BIMATOPROST IN BULK AND OPHTHALMIC DOSAGE FORMS: DEVELOPMENT AND VALIDATION OF AN RP-HPLC METHOD

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (12) ◽  
pp. 49-55
Author(s):  
N. P Ambhore ◽  
◽  
P. M. Dandagi ◽  
A. P. Gadad ◽  
N. H. S. Reddy
Keyword(s):  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Suggested Approach ◽  
Rp Hplc ◽  
System Suitability ◽  
Development And Validation

The main objective of the current study was to develop a simple, accurate, precise and rapid RPHPLC method and subsequent validation using ICH suggested approach for the determination of bimatoprost in bulk and pharmaceutical dosage form. The chromatographic separation of bimatoprost was achieved on a phenomenex C18 column (150 mm × 4.6 mm; 5 μm) using PDA detector at 194 nm. The compound was separated with a mixture of acetonitrile and 0.2% triethylamine (pH 7.0 adjusted with o-phosphoric acid) in the ratio of 50:50 v/v as the optimized mobile phase at the flow rate of 1 mL/min. Chromatogram showed peak of bimatoprost at retention time of 3.8 min. The method was validated for linearity, sensitivity, precision, accuracy, system suitability and robustness. Calibrations were linear over the concentration range of 6.25-100 μg/mL as indicated by correlation coefficient (r2) of 0.999. Developed method can be applicable for routine quantitative determination of bimatoprost in pharmaceutical dosage forms.

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