SPECTROPHOTOMETRIC ESTIMATION AND VALIDATION OF CANAGLIFLOZIN AND METFORMIN HYDROCHLORIDE IN BINARY MIXTURE

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (05) ◽  
pp. 68-72
Author(s):  
Vivek Nalawade ◽  
◽  
Mohammad A. Shaikh ◽  
Vidula Ghodke ◽  
Keyword(s):  
Limit Of Detection ◽  
Spectroscopic Method ◽  
Metformin Hydrochloride ◽  
Simultaneous Estimation ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Uv Visible ◽  
Metformin Hcl

The purpose of the work was to establish a UV spectroscopic method for the simultaneous estimation of canagliflozin and metformin hydrochloride in a binary mix. This method involves interpretation of simultaneous equations based on measurement of absorbance at two wavelengths, 237 nm and 290 nm, using UV-visible spectrophotometer with 1cm matched quartz cells. Methanol solvent was employed in this method. The developed method obeyed Beer’s-Lambert’s law in the concentration range of 2-12 µg/mL, having correlation coefficient 0.9998 and 0.9994 for canagliflozin and metformin hydrochloride, respectively. Different validation parameters like accuracy, precision, limit of detection and limit of quantitation were examined and found to be within the limits. The results of the method were validated as per ICH guidelines. A novel, simple, sensitive, rapid, accurate and economical spectrophotometric methods have been developed for simultaneous estimation of canagliflozin and metformin HCl. The technique can be used to determine the amount of canagliflozin and metformin HCl in a mixture containing canagliflozin and metformin. The absorptivities of canagliflozin and metformin HCl are 0.0481 and 0.0921, respectively. Sandell’s sensitivity (mg/cm2 /0.001 absorbance unit) for canagliflozin and metformin HCl was found to be 0.025 and 0.02931, respectively.

scholarly journals UV Spectrophotometric Methods to Quantify Alogliptin Benzoate and Pioglitazone Hydrochloride

2021 ◽  
pp. 31-41
Author(s):  
Dhanya B. Sen ◽  
Ashim K. Sen ◽  
Aarti S. Zanwar ◽  
Harshita Pandey ◽  
Rajesh A. Maheshwari
Keyword(s):  
Limit Of Detection ◽  
Spectroscopic Method ◽  
Simultaneous Estimation ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
Ich Guidelines ◽  
The Difference ◽  
Tablet Dosage

Three new, precise, accurate and sensitive UV-Spectrophotometric methods namely Ratio Difference Spectroscopic Method (RDSM), First Derivative of Ratio Spectra Method (DR1) and Area Under Curve Method (AUC) were developed and validated for simultaneous assessment of alogliptin benzoate (ALO) and pioglitazone hydrochloride (PIO) in tablet dosage form. In RDSM, ratio spectra of both the drugs were recorded by dividing the mixtures using interfering drug as divisor. Then the difference between the amplitudes of obtained ratio spectra was measured at 288 and 291 nm for ALO and 236 and 245 nm for PIO. The second method DR1, where the first derivative of ratio spectra of both the drugs were recorded and the first derivative signal was measured at 290 nm for ALO and 276.8 nm for PIO. The scaling factor was fixed as 1 and wavelength interval (Δλ) as 2 for recording the first derivative of ratio spectra.  In the third method (AUC), peak area of recorded zero order spectra was measured at 276 ± 10 nm for ALO and 267.8 ± 10 nm for PIO. All three proposed methods were validated according to “International Conference on Harmonization” (ICH) guidelines parameters. For all three methods, ALO and PIO obeyed Beer’s law in the range of 0.5-5 & 1.8-18 µg/ml, respectively. The % RSD of repeatability of measurement, intra-day and inter-day precision were found to be less than 2 for all three methods. Limit of detection (LOD) and Limit of quantification (LOQ) of the drugs were calculated which proved the sensitivity of the methods. The accuracy ranged between 98-101% for all three methods. No interference from pharmaceutical excipients present in the formulation was observed.  These proposed methods were found to be simple, sensitive, accurate and precise and can be applied to the simultaneous estimation of ALO and PIO in combined tablet formulation and also appropriate for routine quality control analysis.

scholarly journals MODIFIED QUANTIFICATION THROUGH HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY ANALYSIS FOR CANAGLIFLOZIN AND METFORMIN HYDROCHLORIDE IN BULK AND TABLETS USING ECOFRIENDLY GREEN SOLVENTS

2017 ◽  
Vol 9 (5) ◽  
pp. 97 ◽  
Author(s):  
Aditya Trivedi ◽  
Noopur Dixit ◽  
D. N. Jhade
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Correlation Coefficient ◽  
High Performance ◽  
Limit Of Detection ◽  
Metformin Hydrochloride ◽  
Simultaneous Estimation ◽  
Green Solvents ◽  
Validation Parameters ◽  
Limit Of Quantitation

Objective: An accurate, precise, specific modified High-Performance Liquid Chromatography method was developed for the simultaneous quantification of canagliflozin and metformin in bulk and dosage forms.Methods: A C18 column (250 x 4.6 mm; 5 µm Phenomenex) was used with mobile phase containing 0.05% v/v triethylamine (pH 6.5): acetonitrile (45:55% v/v) at 20 °C and isocratic pump was used for elution. The flow rate was maintained at 1.2 ml/min and eluents were monitored at 215 nm which is evaluated by sharp peak.Results: The retention times of canagliflozin and metformin were 3.4 min and 12.7 min respectively and showed a good linearity in the concentration range of 40-200 µg/ml of Canagliflozin have found a correlation coefficient of 0.999 and 10-50 µg/ml of Metformin with a correlation coefficient of 0.998. The average percent recoveries were found to be 98.60% and 98.90% respectively for Canagliflozin and Metformin. The developed method follows all the validation parameters like accuracy, precision, linearity, limit of detection, limit of quantitation and solution stability.Conclusion: The proposed method was found to provide faster retention time with sharp resolution with linearity at a lowest concentration as compared to previous methods and this method is validated as per International Conference on Harmonization guidelines and successfully applied to the simultaneous estimation of Canagliflozin and metformin in bulk and dosage forms. There was no such novel method for simultaneous estimation of Canagliflozin and metformin. Hence the developed method is suitable for industrial analysis of Canagliflozin and metformin with eco-friendly,green and less expensive solvents

scholarly journals DEVELOPMENT AND VALIDATION OF A UV SPECTROPHOTOMETRIC METHOD FOR DETERMINATION OF AGOMELATINE IN BULK AND A TABLET DOSAGE FORM

2021 ◽  
Vol 10 (1) ◽  
pp. 22-25
Author(s):  
Firake Bhushan M. ◽  
Pathak Pranjalee V. ◽  
Dorik Pallavi K. ◽  
Siddaiah M.
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Spectroscopic Method ◽  
Uv Spectrophotometry ◽  
Analytical Method Validation ◽  
Analytical Technique ◽  
International Conference ◽  
Validation Parameters ◽  
Limit Of Quantitation

UV spectrophotometry is an analytical technique used routinely for qualitative and quantitative assay due the low cost and reliability during analysis. An simple, efficient, rapid, sensitive, precise and economical UV Spectrophotometric method has been developed for estimation of agomelatine from bulk and pharmaceutical formulation. The method was developed and validated according to International Conference on Harmonization (ICH Q2 R1) guidelines.  The λmax of agomelatine in acetonitrile was found to be 229.6 nm. The analytical method validation parameters linearity, precision, accuracy, robustness were studied according to International Conference on Harmonization guidelines. Pure drug concentration was prepared in the range of 1-10 μg/ml and the linear regression analysis data showed good linear relationship with correlation coefficient value 0.9937. The precision of the method was studied as an intra- day, inter-day variations with value less than 2 % RSD. The limit of detection and limit of quantitation were found to be 0.577 and 1.248 μg/ml, respectively. Recoveries were found to be in the range of 100.815 to 101.744 % and % RSD was less than 2 %. This proposed UV spectroscopic method is simple and suitable for routine analysis. Keywords: Keywords: Agomelatine, Validation, UV Spectrophotometric method

scholarly journals Spectrophotometric Determination of Olmutinib in Bulk by Area under Curve and First Order Derivative Methods and its Validation as per ICH guidelines

2019 ◽  
Vol 9 (4-A) ◽  
pp. 349-354
Author(s):  
BALU KHANDARE ◽  
Atish C. Musle ◽  
Sanket S. Arole ◽  
Pravin V. Popalghat
Keyword(s):  
Area Under Curve ◽  
Limit Of Detection ◽  
Order Derivative ◽  
Spectrometric Method ◽  
First Order ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Limit Of Quantitation

Abstract: A simple, precise and economical UV-spectrophotometric method has been developed for the estimation of Olmutinib from bulk. Two methods were developed First method (A) applied was area under curve (AUC) in which the area was integrated in wavelength from 262-272nm. Second method (B) was first order derivative spectrometric method. In this method absorbance at λmin=256.57nm, λmax=282.83nm and zero cross=267.68nm was measured. Calibration curves were plotted for the method by using instrumental response at selected wavelength and concentration of analyte in the solution. In both the methods, linearity was observed in the concentration range of 2-12µg/ml at the λmax=267.68nm. Accuracy and precision studies were carried out and results were satisfactorily obtained. The drug at each of the 80 %, 100 % and 120 % levels showed good recoveries that is in the range of 98.00 to 99.00% for both methods, hence it could be said that the method was accurate. Limit of detection (LOD) and limit of quantitation (LOQ) were determined for the method. The method was validated as per International Conference on Harmonization. All validation parameters were within the acceptable limit. The developed method was successfully applied to estimate the amount of Olmutinib in pharmaceutical formulation.

scholarly journals A RAPID VALIDATED UNI-DIMENSIONAL DOUBLE DEVELOPMENT HPTLC-DENSITOMETRY METHOD FOR SIMULTANEOUS ESTIMATION OF METFORMIN HYDROCHLORIDE, GLICLAZIDE AND PIOGLITAZONE HYDROCHLORIDE

2019 ◽  
pp. 74-80
Author(s):  
Rajesh Varade ◽  
Harsha Mishra
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Metformin Hydrochloride ◽  
Simultaneous Estimation ◽  
Good Resolution ◽  
Diabetic Medicine ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Layer Chromatography

Objective: To develop and validate a uni-dimensional double development high-performance thin layer chromatography (UDDD-HPTLC) for estimation of anti-diabetic medicine compromising of metformin (MET) gliclazide (GLZ) and pioglitazone hydrochloride (PIO). Methods: The chromatographic separation of these drugs was carried out on precoated TLC plates silica gel 60F254by two mobile phases consisting of Ammonium Sulphate: Methanol: Acetonitrile: Water (4:3:2:1) for MET and PIO and Toluene: Ethyl Acetate: Formic Acid (6:4:0.5) for GLZ respectively for ideal separation and good resolution. The densitometric detection and quantification were carried out at 237 nm for MET and 200 nm for GLZ and PIO. The validation parameters were strictly followed as per the ICH guidelines. Results: The linearity range was obtained at 3000-8000ng/spot, 360-960 ng/spot, 90-240 ng/spot for MET, GLZ and PIO with r2value>0.999. The other parameters such as precision, reproducibility, robustness were efficiently obtained within the limits. The proposed method was successfully applied for simultaneous determination of MET, GLZ and PIO in the commercial formulation. Conclusion: In simultaneous estimation, the different polarity of drugs makes it more cumbersome to develop and validate any chromatographic method. In the present study, a uni-dimensional double development high-performance thin layer chromatography (UDDD-HPTLC) for estimation of these drugs have been developed and validated to resolve the estimation problem. It is an effortless and speedy method which was developed and validated using ICH guidelines. The developed and validated method using ICH guidelines is effortless and speedy technique.

DEVELOPMENT AND VALIDATION OF A UV SPECTROPHOTOMETRIC Q-ABSORBANCE RATIO METHOD FOR SIMULTANEOUS ESTIMATION OF EPERISONE HYDROCHLORIDE AND ACECLOFENAC IN BULK AND TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (11) ◽  
pp. 50-56
Author(s):  
M. Simoes ◽  
◽  
L. Almeida
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Ratio Method ◽  
Simultaneous Estimation ◽  
Absorbance Ratio ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Development And Validation ◽  
Tablet Dosage

A simple, sensitive, rapid, accurate, precise and economical Q-absorbance ratio method has been developed for the simultaneous estimation of eperisone hydrochloride and aceclofenac in combined dosage form. The solvent used was methanol:water (70:30 v/v). The iso-absorptive point was found to be 269.5 nm. Calibration curves were linear over a concentration range of 6-21 μg/ml for eperisone hydrochloride and 8-28 μg/mL for aceclofenac, respectively. The developed method was validated as per International Conference on Harmonization (ICH) guidelines for various parameters such as linearity, precision, accuracy, limit of detection and limit of quantitation. Accuracy of method was determined through recovery studies which were found to be 99.0% - 100.89 % for eperisone hydrochloride and 98.67% - 100.44 % for aceclofenac. Method was found to be reproducible with relative standard deviation (RSD) for intra-and inter-day precision less than 2% over the concentration range. The proposed method can be used for routine analysis of eperisone hydrochloride and aceclofenac in bulk and tablet dosage form.

scholarly journals A Stability Indicating RP-HPLC Method Validation for Simultaneous estimation of Metformin HCl and Canagliflozin in Pharmaceutical Dosage Form

2021 ◽  
pp. 180-192
Author(s):  
Darshak Patel ◽  
Ujashkumar Shah ◽  
Jayvadan Patel ◽  
Hirak Joshi ◽  
Darshana Patel ◽  
...  
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Fixed Dose ◽  
Metformin Hydrochloride ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Validation Parameters ◽  
Metformin Hcl

Aims: Canagliflozin and Metformin HCl is a new drug combination for the treatment of Diabetes Mellitus which is one of the oldest and lethal diseases of the mankind. Aim of the research work was to develop and validate novel, rapid, sensitive, specific, robust stability indicating analytical method for the simultaneous estimation of Canagliflozin and Metformin HCl in the pharmaceutical dosage form as fixed dose formulation. Study Design: Method development and validation was performed as recommended in ICH guideline “Validation of analytical procedures: Test and Methodology Q2(R1)”. Methodology: Method develop with chromatographic parameters as C18 column (250mm×4.6 mm, 5mm particle size), HPLC system with PDA detector and mobile phase contained a mixture of Phosphate Buffer pH 5.0 and Acetonitrile (60:40 v/v). The flow rate was set to 1ml/min with responses measured at 290 nm, injection volume was 20 µl, and run time of 15 mins. Results: The retention time of Metformin Hydrochloride and Canagliflozin was 5.4 min and 7.6 min respectively with resolution of 7.0. Linearity was established in the range of 10-30 µg/ml for Metformin Hydrochloride and 0.5-1.5 µg/ml for Canagliflozin with correlation coefficients more than 0.999. The percentage recoveries were between (98.62-101.22%) and (98.68-101.27%) for Metformin Hydrochloride and Canagliflozin respectively. Validation parameters were evaluated according to the International Conference on Harmonization (ICH) Q2 R1 guidelines. The forced degradation studies were performed by using HCl, NaOH, H2O2, thermal and UV radiation. The developed method was successfully applied for the quantification and hyphenated instrumental analysis. Conclusion: Significance of developed method is that it can be utilize for routine or unknown sample analysis of assay of Metformin HCl and Canagliflozin in pharmaceutical dosage form developed by various Pharmaceutical Industry.

scholarly journals Development and Validation of Estimation of Genotoxic Impurity (Triethyl orthoformate content) in 5-methyl-4-isoxazole carboxylic acid (5-MIA) by using GC Technique

2021 ◽  
Vol 37 (2) ◽  
pp. 348-353
Author(s):  
Mohan bhatale ◽  
Neelakandan kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Gurunathan ramalingam
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Fused Silica ◽  
Triethyl Orthoformate ◽  
Concentration Limit ◽  
Simultaneous Estimation ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Gas Chromatographic Method ◽  
Development And Validation

A simple, selective, precise and accurate Gas chromatographic method for determination of Triethyl orthoformate content (Genotoxic impurity) in 5-MIA is reported. The GC method development and validation as per the International Council for Harmonisation (ICH) guidelines Q2(R1). The effective chromatographic separations were achieved on DB-624, 60 m × 0.53 mm ID, with film thickness of 3.0 μm (Fused silica capillary column), Capillary injector temperature of 150°C, and Nitrogen Carrier gas. This method is unique as there is no UV response; hence GC Method was developed for Triethyl orthoformate. The elution was accomplished with the flow rate of 5.0 mL/min and Split Flow of 10 mL/minute. Detection was performed with FID detector (temp. 260°C) and with column oven temperature program. Methods range from limit of quantitation (LOQ) to 150% level with respect to specification concentration limit of impurity is linear and correlation coefficient of impurity is > 0.99. The linearity of Triethyl orthoformate covered from LOQ to 113 ppm (ie. LOQ to 150% of specification limit) and LOQ to 19 ppm wrt standard concentration. The limit of detection (LOD)values were observed were 2.5 ppm and limit of quantitation (LOQ) were 7.7 ppm, respectively. The parameters selected for the method validated were from international conference on harmonization guidelines, Indian pharmacopeia, USP. The percentage recovery from LOQ, 50% ,100% to 150% level of content were 87.70%, 98.60%, 102.25 and 96.59% respectively. The %RSD values were for LOQ to 150% were from 1.64%, 0.89%, 1.78 % and 1.49%. The range was covered from LOQ to 150% of standard concentration. The results of validation parameters were found in the acceptance range. Standard and sample were stable up to 30 h at when stored at room temperature. Also it was quite robust for the small change in method parameter like, change in column oven temperature(± 5 degree). Hence from the above parameter it was concluded that the GC method with FID detector is selective, precise, linear, and robust for simultaneous estimation of Triethyl orthoformate in Drug Substances.

DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD FOR SIMULTANEOUS ESTIMATION OF ELLAGIC ACID AND BERBERINE IN POLYHERBAL FORMULATION BY RP-HPLC

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (05) ◽  
pp. 52-57
Author(s):  
Pratiksha More ◽  
◽  
Aruna P. Jadhav
Keyword(s):  
Ellagic Acid ◽  
Limit Of Detection ◽  
Low Cost ◽  
Analysis Data ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Polyherbal Formulation ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Development And Validation

An easy, selective, rapid, specific and low cost reverse phase HPLC technique has been developed for the simultaneous estimation of ellagic acid and berberine from a polyherbal formulation. The method was carried out on a Hemochrom Intsil [C18 (250 X 4.6 mm, 5 µ)] column with the mobile phase consisting of methanol: 0.1 % orthophosphoric acid (80:20V/V) at a flow rate of 0.8 mL/min. Detection was carried out at 234 nm. The retention times of ellagic acid and berberine were 4.00 and 2.97 min, respectively. The regression analysis data indicated a good linear relationship for the calibration plots for ellagic acid and berberine in the range of 2-8 µg/mL and 20-80 µg/mL and the regression coefficient was 0.997 and 0.9966, respectively. The accuracy and reliability of the developed method were established by means of comparing numerous validation parameters like linearity, precision, accuracy, robustness, specificity, the limit of quantification and limit of detection, in keeping with the ICH guidelines. The proposed method can be used for the estimation of these markers in other polyherbal formulations.

scholarly journals Development and Validation of Stability Indicating RP-HPLC Method for the Simultaneous Estimation of Dapagliflozin Propanediol and Metformin Hydrochloride in Tablet Dosage Form

2020 ◽  
pp. 660-667
Author(s):  
Nikita Shaileshbhai Patel ◽  
Bhavesh Hirabhai Patel
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Metformin Hydrochloride ◽  
Simultaneous Estimation ◽  
Combination Tablet ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Tablet Dosage

A rapid, precise, accurate, specific and simple stability indicating RP-HPLC method was developed for simultaneous estimation of Dapagliflozin Propanediol (DAPA) and Metformin Hydrochloride (MET) in its tablet dosage form. Method was performed on a column C8 Thermoquest, hypersil division of dimension 250 mm × 4.60 mm having particle size 5 micron. The mobile phase used in the method was 10 mM Ammonium Acetate buffer (pH- 4), Methanol and Acetonitrile in proportion of 30:65:05 respectively. The drug was subjected to acid and alkali hydrolysis, oxidation, photolysis and heat as stress conditions. The method was validated for specificity, linearity, range, precision, accuracy, robustness, LOD, LOQ and system suitability. The flow rate was maintained at 0.8 ml/ min and effluent was monitored at 227 nm. The retention time were observed 5.988 min and 4.661 min for DAPA and MET respectively.  The standard curve was found linear over range of 60-140 μg/ml for DAPA and 300-700 μg/ml for MET with correlation coefficient of 0.9996 for DAPA and 0.9994 for MET. The limit of Detection (LOD) of this method was 1.121 μg/ml for DAPA and 6.162 μg/ml for MET. The limit of Quantitation (LOQ) of this method was 3.396 μg/ml for DAPA and 18.674 μg/ml for MET.  The percentage recovery was found to be in the range of 98-102% at three different levels of a standard addition. The precision (repeatability, intra-day and inter-day) of the method was within the limit (RSD<2%). Degradation products produced because of stress studies did not interfere with the detection of DAPA and MET and the assay can thus be considered stability-indicating. Combination tablet was successfully analysed using the developed method.

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