Chitosan Loaded Mucoadhesive Microspheres of Gliclazide - Journal

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tablet dosage form. For the selection of solvent the criteria employed were sensitivity of the method, ease of sample preparation, solubility of the drug, cost of the solvent and applicability of the method to various purposes. Absorbance of the Entecavir in selected solvent at respective wavelength was determined and molar absorptivity and Sandell's sensitivity was calculated according to the standard formulae (Table 1). Calibration standards Accurately about 100 mg of the pure drug was weighed and dissolved in double distilled water and the volume is made up to the volume 100 ml to give standard stock solution (1000μg/mL) and from this solution 10ml of sample was transferred in to separate 100ml volumetric flask and the volume was made up to the mark 100ml with double distilled water to get concentration 100 µg/ml as a second stock. Aliquots of standard stock solution were pipetted out and suitably diluted with double distilled water to get the final concentration of 2, 4, 6, 8, 10, 12, 14, 16 and 18 μg/ml of standard stock solution. UV-Spectrophotometric method (Method A) Malipatil S.M et al./ Validated UV-Spectrophotometric Estimation of Entecavir in Bulk and Formulations For the selection of analytical wavelength, 10 μg/ml working standard solution was prepared by appropriate dilution of standard stock solution in double distilled water and double distilled water was used as blank solution. This solution was scanned in the spectrum mode from 400 nm to 200 nm. From the spectra of drug (Fig. 2), λ max of Entecavir, 253.6 nm was selected for the analysis. A calibration curve was plotted by taking the absorbance against the concentration of standard stock solutions (Graph 1). By using the calibration curve, the concentration of the sample solution can be determined. First order derivative spectroscopy (Method B) In this method, 10 μg/ml working standard solution was prepared by appropriate dilution of standard stock solution in double distilled water and double distilled water was used as blank solution. This solution was scanned in the spectrum mode from 400 nm to 200 nm wavelength ranges and the first order derivative spectra were obtained at n=1, a sharp peak at 242.6 nm (Fig. 3). The absorbance difference at n=1 (dA/dλ) was calculated, which is directly proportional to the concentration of the standard stock solution. A calibration curve was plotted by taking the absorbance difference (dA/dλ) against the concentration of standard stock solutions (Graph 2). By using the calibration curve, the concentration of the sample solution can be determined. Table 1: Optical characteristics, statistical data of the correlation coefficient and validation parameters for Entecavir by UV spectroscopy, first order derivative & AUC method Parameters Method A Method B Method C λ max 253.6 nm 242.6 nm 258.0-248.0 -1 -1 Molar absorptivity (L mol cm ) Regression equation (Y = a+bc) 4 1.5x10 4 1.108x10 4 3.17x10 Slope(b) 0.0548 0.0040 0.2450 Intercept(a) -0.0007 -0.0002 0.0615 Standard deviation 0.001 0.0004 0.0001 RSD% 0.1824 1.1503 0.00402 2 Correlation coefficient (r ) 0.9999 0.9999 0.9998 Sandell ’ s Sensitivity -2 (µg cm / 0.001 abs unit) % Range of errors 0.003 0.0011 0.0012 Confidence limit with 0.05 level ±0.000788 ±0.000364 ±0.0000788 Confidence limit with 0.01 level Validation parameters ±0.00166 ±0.000539 ±0.000116 Selectivity and Specificity (t-test) 0.305 to 0.290 0.0157 to 0.0255 1.731 to 1.146 Linearity (µg / ml) 2-18 µg/ml 2-18 µg/ml 2-18 µg/ml Limit of detection [LOD] (µg / ml) 0.0601 0.1823 0.001346 Limit of quantitation [LOQ] (µg / ml) 0.1234 0.3740 0.004081 Robustness (mean % recovery ± S.D.) 100.98 ± 0.001 103.41 ± 0.004 101.86 ± 0.0001 Y=bC+a where C is the concentration of Entecavir in µg/ml and Y is absorbance unit. (Each value is a result of nine separate determinations) 112 RJPS, Jul - Sep, 2011/ Vol 1/ Issue 2
Area Under Curve method (Method C) Malipatil S.M et al./ Validated UV-Spectrophotometric Estimation of Entecavir in Bulk and Formulations This method is applicable when there is no sharp peak or when broad spectra are obtained. It involves the calculation of integrated value of absorbance with respect to the wavelength between two selected wavelengths λ 1 and λ 2. Area calculation processing item calculates the area bound by the curve and the horizontal axis. The horizontal axis is selected by entering wavelength range over which the area has to be calculated. This wavelength range is selected on the basis of repeated observations so as to get the linearity between area under 10 curve and concentration. For the selection of analytical wavelength, 10 μg/ml working standard solution was prepared by appropriate dilution of standard stock solution in double distilled water and double distilled water was used as blank solution. This solution was scanned in the spectrum mode from 400 nm to 200 nm (Fig. 4). From the spectra of drug, area under the curve in the range of 258.0-248.0 nm was selected for the analysis. The calibration curve was plotted as AUC against concentration of standard stock solution (Graph 3). By using the calibration curve, the concentration of the sample solution can be determined. ESTIMATION OF ENTECAVIR FROM TABLET DOSAGE FORMS For the estimation of Entecavir in tablet formulation by three methods, 25 tablets of each brand were weighed and triturated to fine powder. Tablet powder equivalent to 25mg of Entecavir was weighed and dissolved and further dilution was carried out with quantity sufficient of double distilled water. This was then filtered through the Whatmann filter paper no. 41 to get the stock solution of concentration 100 Table 2: Accuracy and precision data for the developed methods Level Method A Range (µg/ml) a S.D b % RSD LQC 2.0-4.0 0.0004 0.3071 MQC 8.0-10.0 0.0011 0.2446 HQC Method B 16.0-18.0 0.0008 0.0969 LQC 2.0-4.0 0.00007 0.2551 MQC 8.0-10.0 0.00004 0.3718 HQC Method C 16.0-18.0 0.00003 0.7774 LQC 2.0-4.0 0.000053 0.00659 MQC 8.0-10 0.000149 0.006609 HQC 16.0-18.0 0.000035 0.000839 a b standard deviation, % relative standard deviation LQC Lower Quantifiable Concentration, MQC Middle Quantifiable Concentration, HQC Higher Quantifiable Concentration (Each value is a result of six separate determinations) μg/ml. Further this stock solution was suitably diluted to get 10 μg / ml and these samples were analysed using proposed methods (Table 4). ANALYTICAL VALIDATIONS Specificity and Selectivity Entecavir solutions (10 μg/ml) were prepared in double distilled water along with and without common excipients [lactose monohydrate, microcrystalline cellulose, crospovidone, povidone, and magnesium stearate, titanium Table 3: Results of intermediate precision study Concentration Inter-day repeatability Intra-day repeatability Inter-instrument* (in µg/ml) % RSD (N=8) % RSD (N=8) repeatability % RSD (N=8) Day 1 Day 2 Day 3 Method A 2 0.7932 0.6903 0.4764 0.50 0.73 10 0.1363 0.2140 0.098 2 0.11 0.29 18 Method B 0.0752 0.1181 0.0767 0.10 0.15 2 0.1234 1.3137 1.7788 0.1238 0.62 10 0.2885 3.4077 2.2308 0.2880 0.55 18 Method C 0.9855 1.0137 1.2948 0.9855 0.49 2 0.0279 0.0203 0.0130 0.013 0.021 10 0.0602 0.0466 0.0029 0.002 0.008 18 0.0059 0.0025 0.0026 0.001 0.002 * Instrument 1: Shimadzu UV-Visible spectrophotometer 1700, Instrument 2: Systronic-118 UV-Visible spectrophotometer 113 RJPS, Jul - Sep, 2011/ Vol 1/ Issue 2
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