“DEVELOPMENT AND VALIDATION OF UV SPECTROPHOTOMETRIC METHODS FOR DETERMINATION OF MEGLUMINE IN BULK”

2325 | P a g e J u n e 0 2 , 2 0 1 4 “DEVELOPMENT AND VALIDATION OF UV SPECTROPHOTOMETRIC METHODS FOR DETERMINATION OF MEGLUMINE IN BULK” Barge V. U.*, Jadhav P. B., Attarde S. R., Kodre K. V., Yendhe P.R., Patil R. Y. Pune District Education Associations, Shankarrao Ursal College of Pharmaceutical Science and Research Center, Kharadi, Pune 411 014, India. E-mail:godse_vijaya@rediffmail.com ABSTRACT -


INTRODUCTION
Chemically Meglumine is 1-Deoxy-1-(methylamino)-D-glucitol. It acts as contrast media and it was also used as veterinary anti-inflammatory drug and used in treatment of leishmaniasis and also used as contrast media 1,4 .
The literature survey reveals that Meglumine was analysed by HPLC, NMR spectroscopy was used for determination of Meglumine 2,3 . There are no UV and derivative spectrophotometric methods reported for the analysis of meglumine in bulk. Derivative spectrophotometry is an analytical technique of great utility for extracting both qualitative and quantitative information from spectra composed of unresolved bands, and for eliminating the effect of baseline shift and baseline tilts. It consists of calculating and plotting one of the mathematical derivatives of spectral curve. The derivative spectrophotometry is now a reasonable prized standard feature of modern microcomputerized UV spectrophotometry 6 . The aim of this method was to develop and validate UV calibration curve, first, second and third derivative spectrometric methods for determination of meglumine in bulk.
Analysis is an important component in the formulation development of any drug molecule. It becomes essential to develop a simple, sensitive, accurate, precise, reproducible method for the estimation of drug sample. Our main concern is development and validation of UV, first, second and third derivative spectrometric methods for determination of meglumine in bulk.

Instruments and Material -
The instruments used were UV-1800 UV Spectrophotometer SHIMADZU-120 with UV -1800 UV Spectrophotometer ENG 240V Software. Meglumine pure drug and all chemicals and reagents used were of analytical grade.

Preparation of Standard Stock Solution
Accurately weighed 100 mg of drug was transferred to 100 ml volumetric flask. It was dissolved in 25 ml of distilled water and finally volume was made up to the mark with same solvent to obtain solution of concentration 1000 µg/ml. Then 1ml solution from this solution was transferred in 10 ml volumetric flask and volume was made up to the mark by distilled water to obtain 100 µg/ml 5 .

Determination of λ max for Development of Calibration Curve and Derivative Methods
From the stock solution, 1 ml of meglumine was transferred to 10 ml volumetric flask and the volume was adjusted to the mark with distilled water to obtain strength 10 µg/ml. The solution was scanned in the UV range 200-400 nm.
Determination wavelength for first, second and third derivative The normal UV spectra of λmax 254 nm was derivatised into first, second and third order derivative, using UV probe software of instrument. The amplitude of corresponding troughs was measured at 247 nm, 216 nm, 266 nm.

RESULTS AND DISCUSSION
Validation of method was done as per ICH guidelines.

Linearity
Under the experimental conditions described the graph obtained for UV, first, second and third derivative spectra showed linear relationship. Regression analysis using the method of least-squares was made for the slope. The regression equations of calibration curves were y = 2.2×10 -3 x+7.1×10 -3 , (r = 0.997) for the UV, y =1.2×10 -4 x+2×10 -3 , (r = 0.998) for the first, y = 1×10 -4 x+0.00, (r = 0.997) for the second and y =1×10 -4 x+0.00, (r = 0.997) for the third derivative J u n e 02, 2 0 1 4 spectrophotometric methods, respectively. The range was found to be 10 -60 µg/ml for UV, first, second and third derivative spectrophotometric methods. The statistical parameters given are the regression equation calculated from the calibration graphs, along with the standard deviations of the slope (Sb).

Limit of Detection (LOD) and Limit of Quantification (LOQ)
Limit of detection (LOD) and limit of quantitation (LOQ) were determined by using the formula based on the standard deviation of response and the slope The limit of detection (LOD) and limit of quantification (LOQ) were calculated by using the equations LOD = 3×σ/S and LOQ = 10×σ/S, where σ is the standard deviation, S is the slope (" Table 2")

Precision
To determine the precision of the method, meglumine solutions at a concentration of 40, 50, 60 μg /ml were analyzed each in triplicate. Solutions for the standard curves were prepared fresh every day. The methods were found to be precise. The % RSD values for inter day precision studies were found to be 0.0048, 0.0024, 0.0018 and 0.00031 for UV, first, second and third derivative spectroscopy. The % RSD values for intra day precision studies were found to be 0.00768, 0.00075, 0.01355 and 0.0046 for UV, first, second and third derivative spectroscopy, respectively. The developed methods are accurate, sensitive and precise for determination of meglumine in bulk.

CONCLUSION
This is the first study investigating utility of calibration curve, first order, second order and third order of derivative UVspectrophotometric methods for determination of meglumine in bulk. The proposed methods are correct, precise, sensitive and economic and can be used for the routine analysis and quality control of meglumine.