VOLUME: 09, Special Issue 1, (IC-PRI-2022) Paper id-IJIERM-IX-I, January 2022 4
QUANTITATIVE ESTIMATION OF MEGLITINIDE IN PHARMACEUTICAL DOSAGE FORMS BY UV VISIBLE SPECTROPHOTOMETRY
Kuldeep Vinchurkar*, Sheetal Mane, Jitendra Sainy, Masheer Ahmed Khan, Dinesh K Mishra
Indore Institute of Pharmacy, Indore School of Pharmacy, DAVV, Indore
Abstract - A literal and specific Visible spectrophotometric method was raised for the estimation for Repaglinide in solid pharmaceutical dosage form. The λ-max of Repaglinide was found to be 243nm to both crude and marketed sample and is analysed using Beer-Lamberts law. Beer’s law was obeyed at the concentrations ranging 2-10μg/ml. The developed methods were absolute, definite, explicit and consistent and found to be ap roto type for routine determination for Repaglinide. The method was validated statistically and by recovery studies.
The LOD (limit of detection) and LOQ (limit of quantification) for visible spectra were found to be 0.82μg/ml and1.011μg/ml. The correlation coefficient value was found to be 1.
1 INTRODUCTION
Repaglinide (REP); 2-ethoxy-4-[2-(3-methyl-1- [2-(1-piperidinyl) phenyl] butylamino)-2-oxoethyl]
benzoic acid is a potassium channel blocker fast acting prandial oral hypoglycemic agent for patients with non-insulin-dependent diabetes mellitus1. Repaglinide lowers the fasting glucose concentration by increasing the amount insulin released by the pancreas. It is official in USP
2,3. In the present study, an attempt has been made to develop Visible spectrophotometric method for the determination of Repaglinide in bulk and marketed formulations using methanol4.
Fig. 1 Structure of Repaglinide 2 MATERIALS AND METHODS
UV spectrophotometric method was carried out using Shimadzu 1800 double beam UV ‐ Visible spectrophotometer with UV probe 2.33 software, spectral band width of 2 nm, wavelength accuracy ± 0.5 nm and 1 cm matched pair quartz cells. Repaglinide, a reference standard gift sample from Torrent Pharmaceuticals Limited, Ahmedabda. Eurepa tablet formulations of repaglinide (2 mg) (manufactured by Torrent Pharma. Ltd., Ahmedabad) were purchased from local market. All chemicals and reagents used were of AR/HPLC grade, analytical grade and used without further purification.
2.1 Preparation of Standard Stock Solution
For this, accurately weighed 100 mg of Repaglinde was taken into 100 ml volumetric flask and dissolved into small quantity of methanol (0.1 % w/v). The volume was made up to 100 ml with methanol to get a concentration of (1000 µg/ml) stock solution (SS-I). From this, 10 ml was
VOLUME: 09, Special Issue 1, (IC-PRI-2022) Paper id-IJIERM-IX-I, January 2022 5
withdrawn and diluted with 100 ml of 0.1 N HCl to get a concentration of (100 µg/ml) stock solution (SS-II). From the stock solution (SS-II), 0.2, 0.4, 0.6, 0.8 and 1 ml solutions were withdrawn and transferred into 10 ml volumetric flasks and the final volume was made up with 0.1N HCl to get concentrations of 2 ,4, 6, 8,10 µg/ml respectively. Absorbance of these solutions was recorded at experimental λmax using 0.1 N HCl solution as blank 5,6.
2.2 Determination of max (absorption maxima)
The stock solution (1000µg/ml) was prepared by dissolving 100 mg of Repaglinide in 100 ml methanol. The stock solution was further diluted suitably, with 0.1N HCl to get a working standard solution of concentration of 100 µg/ml. The resulting solution was scanned in the range of 200-400nm on UV-Visible spectrophotometer and the λmax was determined 7.
2.3 Preparation of market sample
To determine the content of repaglinide in conventional tablet. 20 tablets weighed, there mean weight determined and finely powdered 8. A portion of tablet powder equivalent to 10mg of repaglinide was accurately weighed and dissolved in 30 ml methanol in 100 ml volumetric flask and filtered through whattmann filter paper and made up to 60ml with solvent. And the amount of Repaglinide was found by the calibration curve (10μg dilution of drug).
2.4 Recovery Studies
To study the accuracy and reproducibility of the proposed methods, recovery experiments were carried out by adding a known amount of drug to pre analysed sample and the percentage recovery was calculated 9,10.
3 RESULTS AND DISCUSSION
Repaglinide was completely soluble in methanol. Thus, methanol selected as a solvent. The λ max of Repaglinide was found to be 241nm.Linearity was found to be 8-22μg/ml. Correlation coefficient (1) indicate good linearity between concentration and slope area. The method was found to be simple, accurate, and economical for the routine analysis of Repaglinide and its dosage forms. Recovery studies were found to be close to 99.5% that indicated the accuracy and precision of the above proposed method.
3.1 Quantitative Analysis
%Assay = sample absorbance/standard absorbance x100 = 0.639/0.652 x100
= 98.00%
3.2 Molar absorpitivity
ε =E1cm1% x molecular weight /10 4 CONCLUSION
The proposed method was successfully applied for the analysis of Repaglinide in tablet dosage form and method was found to be simple, accurate, economical and rapid. It was observed that excipients did not interfere in the determination of repaglinide. The results obtained by these methods including recovery studies were comparable which proves the repeatability and suitability of the method.
VOLUME: 09, Special Issue 1, (IC-PRI-2022) Paper id-IJIERM-IX-I, January 2022 6
Fig: 2: Determination of Repaglinide by visible spectrophotometry method Fig. 3: calibration curve of Repaglinide
Table 3: Validation parameter Sr no. Parameters Repaglinide
λ-max 243
Beers law limit (ug/ml) 2-10
Correlation coefficient 0.9975
Slope 0.0088
Intercept 0.0013
Regression equation 0.0088x + 0.0013
LOD 0.82
LOQ 1.011
Table 4: Analysis of Repaglinide tablet Drug Label
claim Amount
found (mg) %Label
claim %
Deviation S.D Repaglinide
(Eurepa, Torrent Pharmaceuticals)
10 mg 9.98 99.0 0.232 0.164
Table 5: Recovery studies Sample
added (mg)
Amount of drug recovered (mg)
Amount of drug
Recovered % Mean recovery
1 10 9.82 98.24 100.04
2 10 9.72 97.23 100.03
3 10 9.96 99.62 100.02
VOLUME: 09, Special Issue 1, (IC-PRI-2022) Paper id-IJIERM-IX-I, January 2022 7 REFERENCES
1. Budavari S (2001) The Merck Index. 13th ed. Whitehouse station, (NJ, USA): Merck and Co;1458.
2. Jain SK, Agrawal GP and Jain NK. (2005) Spectrophotometric determination of Repaglinide in tablet dosage form.
Indian J Pharm Sci;67:24951.
3. Goyal A and Singhvi I. (2006) Visible Spectrophotometric Methods for Estimation of Repaglinide in tablet Formulation. Indian J. Pharm. Sci., 68 (5): 656-657
4. Dhole SM, Khedekar PB and Amnerkar ND (2012) Comparison of UV spectrophotometry and high-performance liquid chromatography methods for the determination of repaglinide in tablets. Pharm Methods. Jul-Dec; 3(2): 68–
72.
5. Rajput SJ and Chaudhary BG (2006) Validated analytical technique of Repaglinide in bulk and in tablet formulation. Indian J. Pharm. Sci, 68 (1):130-132
6. 13. Goyal A and Singhvi I. (2006) Visible Spectrophotometric Methods for Estimation of Repaglinide in tablet Formulation. Indian J. Pharm. Sci., 68 (5): 656-657.
7. Patel SR et al (2012) Development and Validation of Analytical Method for Quantitative Estimation of Miglitol and Metformin in Combined Dosage Form. Journal of Applied Pharmaceutical Science. 02 (06): 227-229
8. Makwana M M et al (2012) Simultaneous estimation of Metformin hydrochloride and Repaglinide in pharmaceutical dosage form by UV difference spectrophotometric method. Int Jour Int Pharm And Life Sci.
2(3):38-47.
9. United States Pharmacopoeia 26, NF 21(2003), Rockville M.D, United States Pharmacopoeial Convention Inc.
2440-2443.
10. Sakhreliya BD, Trivedi PD and ModI DK (2012) Development and Validation of Spectrophotometric Methods for Simultaneous Estimation of Escitalopram oxalate and Etizolam in their Combined Tablet. J Pharm Sci Bioscientific Res. 2(5): 195-200
