analytical method development and validation by uv thesis

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• v.2(3); Jul-Sep 2011

Development and validation of the UV-spectrophotometric method for determination of terbinafine hydrochloride in bulk and in formulation

Pritam s. jain.

Department of Pharmaceutical Chemistry, R. C. Patel Institute of Pharmaceutical Education and Research, Shirpur, Dist: Dhule, India

Amar J. Chaudhari

Stuti a. patel, zarana n. patel, dhwani t. patel, background:.

The main objective was to develop and validate the UV-spectrophotometric method for the estimation of terbinafine hydrochloride in bulk and pharmaceutical formulations as per ICH guidelines

Materials and Methods:

A simple, rapid, accurate, and economical UV-spectrophotometric method has been developed for the estimation of terbinafine hydrochloride from bulk and pharmaceutical formulation.

The λ max of terbinafine hydrochloride in water was found to be 283 nm. The drug follows linearity in the concentration range 5–30 μg/ml with a correlation coefficient value of 0.999. The proposed method was applied to pharmaceutical formulation and % amount of drug. estimated was 99.19% and was found to be in good agreement with the label claim. The accuracy of the method was checked by recovery experiment performed at three different levels, i.e., 80%, 100%, and 120%. The % recovery was found to be in the range of 98.54– 99.98%. The low values of % RSD are indicative of the accuracy and reproducibility of the method. The precision of the method was studied as an intraday; interday variations, and repeatability. The % RSD value < 2 indicates that the method is precise. Ruggedness of the proposed method was studied with the help of two analysts.

Conclusion:

The above method was a rapid tool for routine analysis of terbinafine hydrochloride in the bulk and in the pharmaceutical dosage form.

INTRODUCTION

Terbinafine hydrochloride,[ 1 ] ( E )- N -(6,6-dimethyl-2-hepten-4-ynyl)- N -methyl-1-naphthalene methanamine hydrochloride [ Figure 1 ], is a new potent antifungal agent of allylamine class that selectively inhibits fungal squalene epoxidase . The drug is indicated for both oral and topical treatment of mycoses.[ 2 , 3 ] Terbinafine hydrochloride is not yet official in any pharmacopeia, where, only few analytical methods have been reported for its determination in pharmaceutical formulations and biological fluids. Such methods include HPLC,[ 4 – 10 ] colorimetry,[ 11 ] electrochemistry,[ 12 ] and solvent meting method.[ 13 ]

Chemical structure of terbinafine hydrochloride

Among the various methods available for the determination of drugs, spectrophotometry continues to be very popular, because of their simplicity, specificity, and low cost. This study presents a new spectrophotometric method for the determination of terbinafine hydrochloride phosphate in bulk and pharmaceutical formulations. Accordingly, the objective of this study was to develop and validate the UV-spectrophotometric method for the estimation of terbinafine hydrochloride in bulk and pharmaceutical formulations as per ICH guidelines.[ 14 ]

MATERIALS AND METHODS

Terbinafine hydrochloride was a gift sample from Dr. Reddys Lab, Hyderabad. All chemicals and reagents used were of analytical grade and purchased from Qualigens Fine Chemicals, Mumbai, India.

Preparation of standard stock solution

Accurately weighed 10 mg of terbinafine hydrochloride was transferred to a 100 ml volumetric flask, dissolved in 20 ml distilled water by shaking manually for 10 min. The volume was adjusted with the same up to the mark to give the final strength, i.e. 100 μg/ml.

Selection of wavelength for analysis of terbinafine hydrochloride

Appropriate volume 0.5 ml of standard stock solution of terbinafine hydrochloride was transferred into a 10 ml volumetric flask, diluted to a mark with distilled water to give concentration of 5 μg/ml. The resulting solution was scanned in the UV range (200–400 nm). In spectrum terbinafine hydrochloride showed absorbance maximum at 283 nm [ Figure 2 ].

UV spectrum of terbinafine hydrochloride at 283 nm

Validation of the method

The method was validated in terms of linearity, accuracy, precision, and ruggedness.

Linearity study

Different aliquots of terbinafine hydrochloride in the range 0.5–3 ml were transferred into series of 10 ml volumetric flasks, and the volume was made up to the mark with distilled water to get concentrations 5, 10, 15, 20, 25, and 30 μg/ml, respectively. The solutions were scanned on a spectrophotometer in the UV range 200–400 nm. The spectrum was recorded at 283 nm. The calibration plot was constructed as concentration vs . amplitude [ Figure 3 ].

Calibration curve of terbinafine hydrochloride at 283 nm

To the preanalysed sample solutions, a known amount of standard stock solution was added at different levels, i.e. 80%, 100%, and 120%. The solutions were reanalyzed by the proposed method.

Precision of the method was studied as intraday and interday variations. Intraday precision was determined by analyzing the 10, 15 and 20 μg/ml of terbinafine hydrochloride solutions for three times in the same day. Interday precision was determined by analyzing the 10, 15, and 20 μg/ml of terbinafine hydrochloride solutions daily for 3 days over the period of week.

Sensitivity

The sensitivity of measurements of terbinafine hydrochloride by the use of the proposed method was estimated in terms of the limit of quantification (LOQ) and limit of detection (LOD). The LOQ and LOD were calculated using equation LOD = 3.3 × N/B and LOQ = 10 × N/B , where ‘ N ’ is standard deviation of the peak areas of the drugs ( n = 3), taken as a measure of noise, and ‘ B ’ is the slope of the corresponding calibration curve.

Repeatability

Repeatability was determined by analyzing 20 μg/ml concentration of terbinafine hydrochloride solution for six times.

Ruggedness of the proposed method is determined for 20 μg/ml concentration of terbinafine hydrochloride by analysis of aliquots from a homogenous slot by two analysts using same operational and environmental conditions.

Determination of terbinafine hydrochloride in bulk

Accurately weighed 10 mg of terbinafine hydrochloride was transferred into a 100 ml volumetric flask containing 20 ml distilled water, and the volume was made up to the mark using the same. Appropriate volume 0.6 ml of this solution was transferred to a 10 ml volumetric flask, and the volume was adjusted to the mark using distilled water. The resulting solution was scanned on a spectrophotometer in the UV range 200–400 nm. The concentrations of the drug were calculated from linear regression equations.

Application of the proposed method for pharmaceutical formulation

For analysis of commercial formulation 5 ml of terbinafine hydrochloride eye drop solution was taken in a 100 ml volumetric flask and the volume was made up to the mark with distilled water to give 100 μg/ml concentration. From this 2 ml was taken and transferred to a 10 ml volumetric flask and the volume was made up to the mark with distilled water to give 20 μg/ml concentration. It was scanned on a spectrophotometer in the UV range 200–400 nm. The spectrum was recorded at 283 nm. The concentrations of the drug were calculated from the linear regression equation.

RESULTS AND DISCUSSION

Method validation.

The proposed method was validated as per ICH guidelines. The solutions of the drugs were prepared as per the earlier adopted procedure given in the experiment.

Linearity studies

The linear regression data for the calibration curves showed good linear relationship over the concentration range 5–30 μg/ml for terbinafine hydrochloride [ Figure 4 ]. Linear regression equation was found to be Y = 0.0343 X + 0.0294 ( r 2 = 0.999). The result is expressed in Table 1 .

Overlain spectra of terbinafine hydrochloride (5-30 μg/ml) at 283 nm

Linearity study of terbinafine hydrochloride

The solutions were reanalyzed by the proposed method; results of recovery studies are reported in Table 2 which showed that the % amount found was between 98.54% and 99.98% with % RSD > 2.

Recovery studies

The precision of the developed method was expressed in terms of % relative standard deviation (% RSD). These results show reproducibility of the assay. The % RSD values found to be less than 2 that indicate this method precise for the determination of both the drugs in formulation [ Table 3 ].

Precision studies

The linearity equation was found to be Y = 0.0384 X + 0.0314. The LOQ and LOD for terbinafine hydrochloride were found to be 0.42 μg and 1.30 μg, respectively.

Repeatability was determined by analyzing 20 μg/ml concentration of terbinafine hydrochloride solution for six times and the % amount found was between 98% and 102% with % RSD < 2 [ Table 4 ].

Repeatability studies

The peak area was measured for same concentration solutions, six times. The results are in the acceptable range for both the drugs. The results are given in Table 5 . The result showed that the % RSD was less than 2%.

Ruggedness studies

The concentrations of the drug were calculated from linear regression equations. The % amount found was between 99.12% and 100.43% [ Table 6 ].

Analysis of Terbinafine hydrochloride in bulk

The spectrum was recorded at 283 nm. The concentrations of the drug were calculated from the linear regression equation. The % amount found was between 98.24% and 101.31% [ Table 7 ].

Analysis of formulation

This UV-spectrophotometric technique is quite simple, accurate, precise, reproducible, and sensitive. The UV method has been developed for quantification of terbinafine hydrochloride in tablet formulation. The validation procedure confirms that this is an appropriate method for their quantification in the formulation. It is also used in routine quality control of the formulations containing this entire compound.

ACKNOWLEDGMENTS

The authors are thankful to the Principal and Management, R.C. Patel Institute of Pharmaceutical Education and Research, Shirpur (M.S.), India, for providing the required facilities to carry out this research work.

Source of Support: Nil

Conflict of Interest: None declared.

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Analytical Method Development and Validation of UV-Visible Spectrophotometric Method for the Estimation of Saxagliptin in Gastric Medium

Deepika joshi 1 *, bhavana singh 1 , archana rautela 2 and nidhi semwal 1.

1 School of Pharmaceutical Sciences, India

2 Gyani Inder Singh Institute of Professional Studies, India

Submission: March 24, 2021; Published: April 22, 2021

*Corresponding author: Deepika Joshi, School of Pharmaceutical Sciences, SGRRU, India

How to cite this article: Deepika J, Bhavana, Archana R, Nidhi S. Analytical Method Development and Validation of UV-Visible Spectrophotometric Method for the Estimation of Saxagliptin in Gastric Medium. Glob J Pharmaceu Sci. 2020; 8(2): 555735. DOI: 10.19080/GJPPS.2021.08.555735.

Aim: A simple, accurate, precise, cost effective, rapid and sensitive UV/visible spectrophotometric method was developed for the determination of Saxagliptin in active pharmaceutical dosage form. The developed method was validated as per ICH guidelines. Method: The purity of saxagliptin was characterized by solubility profile, melting point, Fourier Transform Infra-Red. The drug was analyzed using UV/visible spectrophotometric method was validated in terms of linearity, accuracy, precision, specificity, Limit of detection and Limit of quantitation. The solvent used was methanol: water (15:85, v/v) and the wavelength corresponding to maximum absorbance of the drug were found at 204 nm. Result: Melting point of drug was found 101°C nearly corresponds to its actual melting range. The linear response for concentration range of 2-10 μg/ml of saxagliptin was recorded with y = 0.1126x - 0.0103, regression coefficient r2 = 0.99068. The accuracy was found between 93.75- 104.16%. Precision for intra-day and inter-day was found to be within the limits. To establish the sensitivity of the method, limit of detection (LOD) and limit of quantification (LOQ) were determined which were found to be 6.77 μg /mL and 20.33 μg /mL respectively. Conclusion: The drug was confirmed by interpretation of UV spectra. Hence proposed method stands out validated and thus may be used for routine analysis of Saxagliptin in pharmaceutical dosage forms.

Keywords: Spectrophotometric method; Saxagliptin; Methanol; Water; Melting point

Abbreviations: UV spectroscopy: Ultraviolet Spectroscopy; ICH: International Conference on Harmonisation; DPP: Dipeptidyl Peptidase; FTIR: Fourier Transform Infra-Red; LOD: Limit of Detection; LOQ: Limit of Quantification

Saxagliptin (SXG) is chemically (1S, 3S, 5S)-2- [(2S)-2-Amino-2-(3 hydroxytricyclo [3.3.1.13,7] dec- 1-yl) acetyl]-2-azabicyclo [3.1.0] hexane-3-carbonitrile previously identified as BMS-477118 as shown in figure 1. The empirical formula is C18H25N3O2.H2O, and the molecular weight is 333.43 [1-4]. Saxagliptin is an oral hypoglycemic or anti-diabetic drug of the dipeptidyl peptidase-4 (DDP-4) inhibitor class. The inhibition of DPP-4 increases levels active of glucagon like peptide 1 (GLP-1), which inhibits glucagon production from pancreatic alpha cells and increases production of insulin from pancreatic beta cells. In 2009, U.S. Food and Drug Administration (FDA) approved saxagliptin and sold under the brand name Onglyza. In adults with type-2 diabetes mellitus, saxagliptin is suggested as an add-on to diet and exercise to improve glycemic control [5-11].

Literature survey reveals that the drug can be estimated only by LC-MS/MS, spectrophotometric method have been reported [12,13]. The aim of the present work was to develop a simple, sensitive, precise and accurate UV/Visible spectrophotometric method for the determination of saxagliptin in its pure form and pharmaceutical formulations further, to validate the developed method.

Chemical and reagents

All the chemicals used were of analytical grade. All the solutions were freshly prepared in Methanol and 0.1N HCl (15:85, v/v). Authentic of saxagliptin were obtained as gift samples from Mylan Laboratories Limited, Hyderabad

Saxagliptin was estimated using UV-Visible spectrophotometer (Shimadzu model 1800 double beam) at the wavelength of maximum absorption (204 nm) in acidic medium containing 0.1N HCl. The drug was characterized by solubility, melting point, and Fourier Transform Infra-Red (FTIR) techniques. The analysis of the drug was carried out by UV-Visible method which was validated analytical parameters like linearity, precision, and accuracy as per guidelines laid down by International Conference on Harmonization (ICH).

Physical characterization of saxagliptin

The physical characterization of procured drug sample of saxagliptin was determined on the basis of following parameters.

Organoleptic properties

The organoleptic properties have been determined for nature, colour, taste and odour of the pure sample of saxagliptin

Excess amount of saxagliptin was dissolved in 10 ml distilled water till a saturated solution was obtained. The saturated solution of saxagliptin was stirred for 48 hrs on magnetic stirrer at 100rpm and room temperature (at 25 ± 1ºC). Then the sample was centrifuged for 10 min at 10,000 rpm. Clear supernant was collected using 0.22 μm syringe filter and analysed using UV spectrophotometer. The results were analysed and noted [14].

Melting point

Melting point of saxagliptin was determined using capillary melting point apparatus. In this method a small quantity of drug was filled in a capillary tube open both the ends and it was placed along with thermometer in melting point apparatus.

Fourier transform Infrared spectroscopy (FTIR)

FTIR spectrum was used as an analytical technique for identification of pure drug sample by KBr method using FTIR spectrometer (Agilent Technologies, USA). Peaks of individual pure drug were compared with reference FTIR peaks. Samples were previously prepared with KBr at 1: 5 (sample: KBr, w/w). KBr disks were prepared by compressing the powders at a pressure of 5 tons for 3 min in a hydraulic press and scanned against a blank KBr disk at wave numbers ranging from 500 to 4000 cm-1 with a resolution of 1.0 cm-1 [15].

Analytical method for drug concentration measurements (UV/Visible method)

The ultraviolet spectrophotometric method was selected for the estimation of saxagliptin in the range of 200 to 400 nm and the λmax was determined.

Diluent preparation

Methanol and 0.1N HCl (15:85, v/v) were used as a diluents.

Preparation of saxagliptin stock solution (20μg/ml) in 0.1N HCl

Saxagliptin was weighed equivalent to 100mg and transferred into 100ml volumetric flask then 15ml of methanol was added and shaked well to dissolve it after that the volume was made up to 100ml with 0.1N HCl. From that 2ml of solution was withdrawn and taken in 100ml volumetric flask. The volume was adjusted with diluent up to up to 100ml with 0.1N HCl [16,17] as shown in table 1.

Selection of detection wavelength

Drug solution was scanned over the range of 200- 400 nm. The wavelength of saxagliptin was determined to be 204 nm.

Preparation of working standard

Prepare a series of dilute solution from the above stock solution according to table 2 in 10 ml volumetric flask. Measure the absorbance of the solutions at 204 nm using distilled water as a blank. Plot a graph by taking concentration (μg/ml) on X-axis and absorbance on Y-axis. This plot gives a straight line and the linearity can be determined using y = mx + C formula. From the calibration curve calculate the Coefficient of determination R2 value, slope m and intercept C using the following formula, OR by excel sheet.

Construction of calibration curve

Pipette out 1,2,3,4,5,6,7, and 8 ml of working solution and transfer into separate 10 ml volumetric flasks. Dilute all of them to 10 ml with water to get solution of concentrations to 2, 4, 6,8,10,12,14,16 μg/ml respectively

Appropriate aliquots of saxagliptin working standard solutions were taken in different 10 ml volumetric asks and diluted up to the mark with distilled water to obtain final concentrations of 2, 4, 6, 8, 10 μg/ml. Calibration curves were constructed by plotting absorbance versus concentrations and regression equations were calculated for both the drugs.

The Range of the analytical method was decided from the interval between the upper and lower level of the calibration curve by plotting curve.

Intraday precision was determined by analyzing the drugs at concentrations (4μg/mL) and each concentration for three times, on the same day. Inter-day precision was determined similarly, but the analysis is carried out daily, for two consecutive days. Repeatability (intraday) of the method was determined by analyzing six samples of the same concentrations of the drug (4μg/mL). The absorbance of each was measured and reported in terms of relative standard deviation to obtain the variation.

The accuracy of the method was determined by calculating recoveries of saxagliptin by method of standard additions at three different levels 60, 100 and 140 %. Mean percentage recovery was determined. Recovery values were calculated and shown in table 1.

Detection limit

The Detection Limit of an individual analytical procedure is the lowest amount of analyte in a sample which can be detected but not necessarily quantitated as an exact value. The detection limit (LOD) may be expressed as. LOD= 3.3σ/S Where σ = Relative standard deviation of the response. S = the slope of the calibration curve (of the analyte).

The Quantitation limit of an analytical procedure is the lowest amount of analyte in a sample, which can be quantitatively determined with suitable precision and accuracy.

Quantitation Limit (LOQ) may be expressed as: LOQ = 10σ/S Where

σ = Relative standard deviation of the response.

S = the slope of the calibration curve (of the analyte).

Saxagliptin was found to be white colored, non-hygroscopic, crystalline powder.

The solubility of saxagliptin in water was found to be 2.12 ± 0.28 mg/L corresponding to reference value of 2.9 mg/L.

Fourier transform infrared spectroscopy (FTIR)

FTIR spectrum for identification of pure drug sample was done by FTIR spectrometer. Major absorption peaks of saxagliptin was found at 3450.12 cm-1 (N-H stretching), 2912.61 cm-1 (C-H stretching), 3301 cm-1 (OH stretching), 1614.47 cm-1 (C-N stretching), 1255.70 cm-1 (C-O stretching) as shown in figure 2 which corresponds to the literature peaks confirming the purity of drug sample.

The melting point was determined by capillary melting point apparatus. The observed melting point of saxagliptin is 101°C

Analytical method for drug concentration measurements (UV/VIS Method)

Selection of detection wavelength: The wavelength of saxagliptin was determined to be 204 nm as shown in figure 3.

Preparation of standard plot for saxagliptin: Absorbance of the resultant solution was measured at 204 nm using blank. A graph was plotted between the concentrations and their respective absorbance. The response of the drug was found linear in the entire investigational range of 2 to 10μg/ml as shown in table 1. The calibration curve showed the linear equation as, y = 0.1126x - 0.0103, with a correlation coefficient, r2 = 0.99068, where y represents absorbance (optical density) and x represents the concentration (μg /ml) as shown in figure 4.

Method validation: The developed method was validated as per ICH guidelines for the following parameters:

Linearity: The linearity for Saxagliptin was found to be linear in the range of 2-10 μg/ml. The regression equation was found to be y = 0.1126x - 0.0103, r2 = 0.99068.

Range: The observed range of saxagliptin in test solution was observed from 0.097± 0.0005 to 0.871± 0.001.

Accuracy: The accuracy of the analytical method for Saxagliptin was determined at 60%, 100% and 140% levels of standard solution. Absorbance was measured at 204 nm and results were expressed in terms of % recoveries in table 2.

Precision: The Intra-day and Inter-day precision were carried out using same optimized conditions. The precision (measurement of inter-day, intra-day repeatability) results showed good reproducibility with the relative standard deviation (% RSD) below 2.0 % as shown in table 3 & 4 respectively. This indicated that the method was highly precise.

Limit of detection (LOD) and limit of quantification (LOQ): LOD and LOQ of method were determined to be 6.77 μg /mL and 20.33 μg /mL respectively. LOD and LOQ indicate that method was highly sensitive and fast.

The method was validated and found to be simple, sensitive, accurate and precise as per ICH guidelines [21]. The % RSD for the validation parameters was found to be less than 2%. Hence proposed method may be used for routine analysis of these drugs in pharmaceutical dosage forms. Accuracy of proposed method was confirmed by performing accuracy studies that showed the results within the range. Precision of proposed UV method was confirmed by performing intra-day and inter-day precision. Results were well within acceptance criteria that indicate excellent scope of the method for the determination of Saxagliptin in pharmaceutical dosage forms and bulk.

All authors have contributed significantly in the preparation of the manuscript and are in agreement with the content of the manuscript and agree to submission to Global Journal of Pharmacy & Pharmaceutical Sciences, Juniper Publishers. Authors are grateful to Mylan Laboratories Limited, Hyderabad for providing the gift sample. The authors express gratitude to School of Pharmaceutical Sciences, SGRRU, Dehradun.

The authors declare that there is no conflict of interest that could be prescribed as prejudging the impartiality of the review. This research did not receive any specific grant from funding agencies in the public, commercial, or not-for-profit sectors.

This work did not receive any specific grant from funding agencies in the public, commercial, or not-for-profit sectors.

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Analytical Method Development and Validation of UV-visible Spectrophotometric Method for the Estimation of Vildagliptin in Gastric Medium

Affiliation.

• 1 Department of Pharmacy, School of Medical and Allied Sciences, GD Goenka University, Gurugram, Haryana, India.
• PMID: 32746479
• DOI: 10.1055/a-1217-0296

Background: Vildagliptin is an antidiabetic agent, belongs to the dipeptidyl peptidase IV (DPP-4) inhibitors.

Objective: The aim of investigation was to develop a simple UV-visible Spectrophotometric method for the determination of vildagliptin in its pure form and pharmaceutical formulations, further to validate the developed method.

Material and methods: Vildagliptin was estimated using UV-Visible double beam spectrophotometer at the wavelength of maximum absorption (210 nm) in acidic medium containing 0.1N HCl. The drug was characterized by melting point, Differential Scanning Calorimetry (DSC), and Fourier Transform Infra-Red (FTIR) techniques. The analysis of the drug was carried out by novel UV-Visible method which was validated analytical parameters like linearity, precision, and accuracy as per guidelines laid down by International Conference on Harmonization (ICH).

Result: Melting point of drug was found 154°C which is corresponds to its actual melting range. Similarly by the interpretation of spectra the drug was confirmed. The linear response for concentration range of 5-60 µg/ml of vildagliptin was recorded with regression coefficient 0.999. The accuracy was found between 98-101%. Precision for intraday and interday was found to be 1.263 and 1.162 respectively, which are within the limits. To establish the sensitivity of the method, limit of detection (LOD) and limit of quantification (LOQ) were determined which were found to be 0.951 µg/ml and 2.513 µg/ml respectively.

Conclusion: The UV method developed and validated for vildagliptin drug was found to be linear, accurate, precise and economical which can be used for the testing of its pharmaceutical formulations.

© Georg Thieme Verlag KG Stuttgart · New York.

• Acids / chemistry*
• Calorimetry, Differential Scanning / methods
• Hypoglycemic Agents / chemistry*
• Limit of Detection
• Reproducibility of Results
• Spectrophotometry, Ultraviolet / methods
• Vildagliptin / chemistry*
• Hypoglycemic Agents
• Vildagliptin

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