VALIDATED RP-HPLC AND UV-SPECTROSCOPY METHODS FOR THE ESTIMATION OF DAPAGLIFLOZIN IN BULK AND IN TABLETS

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (03) ◽  
pp. 44-51
Author(s):  
B. Sabbagh ◽  
B. V. S. Lokesh ◽  
G. A. Akouwah ◽  
Keyword(s):  
Good Accuracy ◽  
Uv Spectroscopy ◽  
Linear Regression Analysis ◽  
Molar Absorptivity ◽  
Hplc Method ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Significant Difference ◽  
Uv Visible

Two methods were developed for the determination of dapagliflozin (DAPA) in pure form and in tablets. The procedure utilized was UV-Visible Spectroscopy and RP-HPLC with PDA detector to quantify DAPA in bulk and tablets. The sensitive linear range was identified for both methods within 0.5-5.0μg/mL. The linear regression analysis was identified for both methods with correlation coefficient(r)>0.99. The LOD and LOQ values were found to be 0.05 μg/mL and 0.5 μg/mL for the method by UV-Spectroscopy. The molar absorptivity (ε) was calculated as 1.27 X 105 L.mol-1cm-1. The RP-HPLC method produced LOD and LOQ values of 1.0 ng/mL and 0.5 μg/mL. Both methods were simple, precise, reproducible to quantify the amount of unknown in bulk as well as in tablets and estimated accurately within the range of 100.0±0.5%. Statistical analysis was performed on the data obtained. There was no significant difference between the developed and reported methods with p>0.05. Both methods can be applied for routine analysis of DAPA in bulk and tablets with good accuracy and precision.

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

scholarly journals New Application of Chromotropic Acid for the Determination of Some Sulphonamides in their Pharmaceutical Preparations

2002 ◽  
Vol 70 (1) ◽  
pp. 49-55
Author(s):  
Abou-Attia Fekria M. ◽  
Issa Y.M. ◽  
El Reis M.A. ◽  
Aly F.A. ◽  
Abd El- MoetY M.
Keyword(s):  
Azo Dye ◽  
Good Accuracy ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Extraction Process ◽  
Molar Absorptivity ◽  
Chromotropic Acid ◽  
Time Consumption ◽  
Accuracy And Precision

The formation of the azo-dye using chromotropic acid as a coupling agent was applied to the determination of five sulphonamides. The spectrophotometric studies as well as microanalysis of the studied sulphonamides- chromotropic acid azo dyes revealed the existence of the 1:1 coupling product. The absorbance of the formed azo dye is measured at 510 nrn, and has a large molar absorptivity (ε = 2.87 - 3.29 × 104 1 mol−1cm−1). Beer's law was obeyed over the concentration range 0.5-9.0 µg ml−1. The assay results of pharmaceutical formulations showed good accuracy and precision over the concentration range used. The proposed method avoids time-consumption, extraction process and temperature control.

scholarly journals Spectrophotometric and RP-HPLC Methods for Determining Cefotaxime Sodium in Pharmaceutical Preparations

2020 ◽  
Vol 32 (6) ◽  
pp. 1314-1320
Author(s):  
Lamya A. Sarsam ◽  
Salim A. Mohammed ◽  
Sahar A. Fathe
Keyword(s):  
Limit Of Detection ◽  
Phosphate Buffer Solution ◽  
Pharmaceutical Preparations ◽  
Molar Absorptivity ◽  
Hplc Method ◽  
Buffer Solution ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Relative Standard

A rapid, simple and sensitive spectrophotometric and RP-HPLC methods have been developed for the quantitative determination of cefotaxime-Na in both pure and dosage forms. The spectrophotometric method was based on diazotization of cefotaxime-Na and then coupling with 8-hydroxyquinoline in an alkaline medium. The resulting azo dye exhibited maximum absorption at 551 nm with a molar absorptivity of 0.597 × 104 L mol-1 cm-1. Beer′s law was obeyed over the range 10-700 μg/25 mL (i.e. 0.4-28.0 ppm) with an excellent determination coefficient (R2 = 0.9993). The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.0194 and 0.3765 μg mL-1, respectively. The recoveries were obtained in the range 97.3-102.5% and the relative standard deviation (RSD) was better than ± 1.56. The HPLC method has been developed for the determination of cefotaxime-Na. The analysis were carried out on a C18 column and a mobile phase composed of acetonitrile and phosphate buffer solution (0.024M KH2PO4 and 0.01M H3PO4) at pH 3.5 in the ratio of 60:40 (v:v), with a flow rate of 1.0 mL min-1 and UV detection at 258 nm. The proposed method showed good linearity (in a range of concentration 1.0-200 μg mL-1. The recovery percent and a relative standard deviations were found in the range 96 to 104.8% and ± 0.017 to ± 0.031%, respectively. Both methods were applied successfully to the assay of cefotaxime-Na in commercial injection preparations.

A Validated HPLC Method for Simultaneous Determination of Perindopril Arginine, Amlodipine, and Indapamide: Application in Bulk and in Different Pharmaceutical Dosage Forms

2017 ◽  
Vol 100 (4) ◽  
pp. 992-999 ◽  
Author(s):  
Ramzia I El-Bagary ◽  
Ehab F Elkady ◽  
Shereen Mowaka ◽  
Maria A Attallah
Keyword(s):  
Potassium Dihydrogen Phosphate ◽  
Pharmaceutical Preparations ◽  
Dosage Forms ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Pharmaceutical Dosage Forms ◽  
Potassium Dihydrogen ◽  
Accuracy And Precision ◽  
Significant Difference

Abstract A simple, accurate, and precise LC method with a reversed stationary phase was developed and validated for the determination of perindopril (PER) arginine, amlodipine (AML), and indapamide (IND) alone and in binary mixtures (PER arginine is found in two dosage forms, i.e., with either AML or IND). Chromatographic separation was carried out on a BDS Hypersil® C18 column (100 × 3 mm, 5 μm). The mobile phase, consisting of 0.05 M potassium dihydrogen phosphate buffer (pH 2.6)–methanol (50 + 50, v/v), was pumped through the column whose temperature was maintained at 50°C at a flow rate of 0.6 mL/min using isocratic elution, and UV detection at 215 nm was performed. Acceptable values of linearity, accuracy, and precision of the method were found over the concentration ranges of 5–80 μg/mL PER, 2.5–80 μg/mL AML, and 0.5–20 μg/mL IND. The proposed chromatographic method was statistically compared to that of reference methods using one-way analysis of variance. The results showed that there was no significant difference between the methods. The developed method proved reliable for use in accurate QC of the drugs in their pharmaceutical preparations.

Selective determination of tantalum in ores by extraction with N-phenylbenzohydroxamic acid in toluene

1990 ◽  
Vol 55 (7) ◽  
pp. 1686-1690 ◽  
Author(s):  
José Aznarez ◽  
Juan Carlos Vidal ◽  
Cecilia Vaquero
Keyword(s):  
Hydrochloric Acid ◽  
Acid Solution ◽  
Aqueous Phase ◽  
Spectrophotometric Determination ◽  
Absorption Maximum ◽  
Good Accuracy ◽  
Molar Absorptivity ◽  
Selective Determination ◽  
Accuracy And Precision

A method for tantalum(V) spectrophotometric determination in a non-aqueous phase is proposed. Tantalum(V) is extracted with N-phenylbenzohydroxamic acid into toluene from a 5M hydrochloric acid solution. The colour is then developed by addition of 4-(2-pyridylazo)-resorcinol (PAR) solution in N,N-dimethylformamide and pyridine to an aliquot of the extracted phase. The Ta(V)-PAR complex gives an absorption maximum at 547 nm with a molar absorptivity of 3.88 ± 0.04 . 104 l mol-1 cm-1. The method has been applied to the selective determination of tantalum in ores with good accuracy and precision.

Stability-Indicating TLC-Densitometric and HPLC Methods for the Simultaneous Determination of Piracetam and Vincamine in the Presence of Their Degradation Products

2016 ◽  
Vol 99 (6) ◽  
pp. 1490-1498 ◽  
Author(s):  
Amal B Ahmed ◽  
Maha M Abdelrahman ◽  
Nada S Abdelwahab ◽  
Fathy M Salama
Keyword(s):  
Simultaneous Determination ◽  
Degradation Products ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Array Detection ◽  
Assay Methods

Abstract Newly established TLC-densitometric and RP-HPLC methods were developed and validated for the simultaneous determination of Piracetam (PIR) and Vincamine (VINC) in their pharmaceutical formulation and in the presence of PIR and VINC degradation products, PD and VD, respectively. The proposed TLC-densitometric method is based on the separation and quantitation of the studied components using a developing system that consists of chloroform–methanol–glacial acetic acid–triethylamine (8 + 2 + 0.1 + 0.1, v/v/v/v) on TLC silica gel 60 F254 plates, followed by densitometric scanning at 230 nm. On the other hand, the developed RP-HPLC method is based on the separation of the studied components using an isocratic elution of 0.05 M KH2PO4 (containing 0.1% triethylamine adjusted to pH 3 with orthophosphoric acid)–methanol (95 + 5, v/v) on a C8 column at a flow rate of 1 mL/min with diode-array detection at 230 nm. The developed methods were validated according to International Conference on Harmonization guidelines and demonstrated good accuracy and precision. Moreover, the developed TLC-densitometric and RP-HPLC methods are suitable as stability-indicating assay methods for the simultaneous determination of PD and VD either in bulk powder or pharmaceutical formulation. The results were statistically compared with those obtained by the reported RP-HPLC method using t- and F-tests.

scholarly journals Development and Validation of RP-HPLC Method for Estimation of Amlodipine Besylate and Celecoxib in Pharmaceutical Formulation

2020 ◽  
Vol 10 (6) ◽  
pp. 31-36
Author(s):  
P Nagamani ◽  
SY Manjunath ◽  
T Hemant Kumar
Keyword(s):  
High Performance ◽  
Pharmaceutical Products ◽  
Hplc Method ◽  
Amlodipine Besylate ◽  
Linear Calibration ◽  
Rp Hplc ◽  
Uv Visible ◽  
Development And Validation ◽  
Tablet Dosage

A simple, precise, accurate, and rapid reverse phase-high performance liquid chromatography (RP-HPLC) method with UV-Visible detector has been developed and subsequently validated for the simultaneous determination of amlodipine besylate(AML) and celecoxib(CEL) in their combined tablet dosage form. The separation was based on the use of a Flowrosil C18   analytical column (250 × 4.6 mm, i.d., 5 µm). The mobile phase consisted of a mixture of 80 volumes of acetonitrile and 20 volumes of water. The chromatography was performed by isocratic elution at a flow rate of 1 mL/min. Analytes were detected at 250 nm, with linear calibration curves at concentration ranges of 2-12 µg/ml and 50-300 µg/ml for AML and CEL respectively. The retention time of AML and CEL were 1.98 and 3.15 min respectively. The recoveries obtained were 99.46‒101.36% for AML, 99.57‒101.42% and 99.96–100.87 % for CEL. The method was validated according to International conference of harmonisation guidelines in terms of accuracy, precision, specificity, robustness, limits of detection and quantitation, and other aspects of analytical validation. The developed method was applied successfully for HPLC analysis of commercial pharmaceutical products including AML and CEL. Keywords: Amlodipine besylate; Celecoxib; RP-HPLC.

scholarly journals Stability Indicating RP-HPLC Method For Determination Of Ketoconazole In Bulk Drug And In Tablet Dosage Form

2021 ◽  
Vol 001 (02) ◽  
Author(s):  
Shalin Parikh ◽  
Jayant Dave ◽  
Jayendrakumar Patel
Keyword(s):  
Dosage Form ◽  
Linear Regression Analysis ◽  
Hplc Method ◽  
Stress Conditions ◽  
Dihydrogen Phosphate ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Bulk Drug

A simple, precise, accurate and sensitive isocratic stability indicating RP-HPLC method has been developed and validated for determination of Ketoconazole in bulk drug and pharmaceutical dosage form. Isocratic RP-HPLC separation was achieved on Agilent C8 (150 mm ?4.6 mm, 5 µm particle size) with the mobile phase 0.3 % Triaethylamine in 20 mM potassium dihydrogen phosphate buffer pH adjusted to 4.0: Acetonitrile (68:32 % v/v) at a flow rate 1.0 ml/min. The retention time of Ketoconazole was 8.97 ± 0.50 min. The method was validated for specificity, linearity, precision, accuracy and robustness. The linear regression analysis data of calibration curve showed good linearity in concentration range 10-60 ?g/ml. The Intraday and Interday precision were 0.59-1.11 % and 0.26-1.73 % RSD respectively. The accuracy was found to be 98.11-99.26 %. The drug was subjected to the stress conditions like hydrolysis, oxidation, photolysis and dry heat. The proposed method is found to be specific with respect to degradation product formed after Acidic hydrolysis, Oxidation, Thermal and Photolytic degradation. The Ketoconazole was found to be stable under neutral hydrolytic, thermal and photolytic stress conditions. Acidic, thermal, photolytic stress conditions showed degradation. The proposed chromatographic method can be used for estimation of drug during stress testing & formal stability studies.

scholarly journals Simultaneous Determination of Piracetam and Citicoline in Combination Drug Products by Rp-Hplc Method

2021 ◽  
pp. 171-185
Author(s):  
Meka. Srinivasa Rao ◽  
K. Rambabu
Keyword(s):  
Hplc Method ◽  
Simultaneous Estimation ◽  
Combination Drug ◽  
Drug Products ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
System Suitability ◽  
Relative Standard

In this paper a simple, accurate and precise RP-HPLC method for the simultaneous. Estimation of piracetam and citicoline in synthetic mixtures has been developed and validated. Separation of drugs was carried out using buffer and Acetonitryle with proportion of 60:40 %v/v as mobile phase at 5 min. run time and 265nm. The Rt value for piracetam and citicoline was found to be 3.158 and 5.196 min respectively. The developed method has been validated for linearity, accuracy and precision, LOD, LOQ, and system suitability according to ICH guidelines. The low values of LOD and LOQ illustrate that the developed method was sensitive, accurate, and precise as it can detected and quantify with very low concentration. The low % RSD values below 2 indicate that the method is precise. The above validation studies revealed the method is specific, rapid, reliable, and reproducible. The high recovery and low relative standard deviation confirm the suitability of the method for routine determination of piracetam and citicoline in combined dose products.

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