A New Validated Third Order Derivative Spectroscopic Method For Simultaneous Estimation Of Metoprolol Succinate And Ramipril In Tablet Dosage Form

Objective: The objective of the present work is to develop and validate a new UV derivative spectrophotometric method for simultaneous estimation of metoprolol succinate and ramipril in methanol: water (50:50v/v). Methods: “Zero crossing technique” was chosen for quantitative determination. The zero-crossing points (ZCP’s) were found to be 209 nm where metoprolol succinate was quantified and 211 nm where ramipril was quantified. This method was then subjected to accuracy, linearity, sensitivity and reproducibility according to ICH guidelines to ensure and confirm its validity. Results: The method was found to be obeying Beer’s law in the range of 10-50 µg/ml and 5-25 µg/ml for metoprolol succinate and ramipril, respectively. The % recoveries were observed between the range of 99.2-100.2 for metoprolol succinate and 99.57-99.86 for ramipril. The intra-day and inter-day results showed reproducibility. Conclusion: It can be concluded that the developed third-order UV derivative spectroscopic method for the simultaneous determination of metoprolol succinate and ramiprilcan be recommended for routine quantitative analysis.

Quantitative Analysis Of Pamabrom And Ibuprofen In Synthetic Mixture Using 1st Order Derivative Spectroscopy

Objective: The preliminary goal was to develop and validate 1st order derivative spectroscopic method for quantitative analysis of Pamabrom (PAMA) which is a xanthine diuretic and ibuprofen (IBU) which is a non-steroidal anti-inflammatory agent from its synthetic mixture. Methods: Analytical method was developed on Shimadzu double beam spectrophotometer equipped with UV probe 2.42 as software using methanol as solvent. Quantification of PAMA was carried out at zero cross over point of IBU that is 291 nm and for IBU, it was achieved at 278 nm which is zero cross over point of PAMA. Method was validated according to ICH Q2 R1 guidelines. Results: Method showed a linear response in the range of 2-12 µg/ml of PAMA and 20-120 µg/ml of IBU. Method was found to be accurate with recovery between 99.7–100.9 % for PAMA and 100.3–100.7 % for IBU. The method was found to be accurate and precise for quantitative analysis of PAMA and IBU. Conclusion: The developed method was successfully validated as per ICH Q2 R1 guidelines and was successfully applied for quantitative analysis of a synthetic mixture of PAMA and IBU.

A comparative study of two separate analytical techniques for the simultaneous determination of diclofenac sodium and diacerein from combined dosage form

ABSTRACT Diclofenac sodium (DS) and diacerein (DC) have emerged as a potential combination therapy for the treatment of knee osteoarthritis. Therefore a validated analytical method is essential for the simultaneous estimation of both from combined dosage form. A ratio derivative spectrophotometric and a chromatographic technique have been developed for the simultaneous determination of DS and DC. The quantification was done at 263.00 nm for DC and 304.50 nm for DS in the first method, whereas 257 nm for DC and at 274 nm for DS for LC-DAD analysis in chromatographic method using acetate buffer and methanol as the mobile phase at a flow-rate 0.50 mL/min. Both of these methods are found to be linear in the concentration range under study with r2 value 0.999 and 0.996 for DS and DC respectively in ratio derivative spectroscopy and 0.998 and 0.999 for DS and DC respectively in LC-DAD study. Both of these methods are found to be accurate and precise, though greater robustness and precision is observed with chromatographic analysis over the ratio derivative spectroscopy. Statistically there was no significant difference between proposed ratio derivative spectrophotometric and LC-DAD methods.

Transmission FTIR derivative spectroscopy for estimation of furosemide in raw material and tablet dosage form

A Fourier transform infrared derivative spectroscopy (FTIR-DS) method has been developed for determining furosemide (FUR) in pharmaceutical solid dosage form. The method involves the extraction of FUR from tablets with N,N-dimethylformamide by sonication and direct measurement in liquid phase mode using a reduced path length cell. In general, the spectra were measured in transmission mode and the equipment was configured to collect a spectrum at 4 cm(-1) resolution and a 13 s collection time (10 scans co-added). The spectra were collected between 1400 cm(-1) and 450 cm(-1). Derivative spectroscopy was used for data processing and quantitative measurement using the peak area of the second order spectrum of the major spectral band found at 1165 cm(-1) (SO2 stretching of FUR) with baseline correction. The method fulfilled most validation requirements in the 2 mg/mL and 20 mg/mL range, with a 0.9998 coefficient of determination obtained by simple calibration model, and a general coefficient of variation <2%. The mean recovery for the proposed assay method resulted within the (100±3)% over the 80%-120% range of the target concentration. The results agree with a pharmacopoeial method and, therefore, could be considered interchangeable.

Analytical method development and validation of sitagliptine phosphate monohydrate in pure and tablet dosage form by derivative spectroscopy.

In this study zero, first and second order derivative spectrophotometric method were developed for the estimation of sitagliptine. In zero order spectrophotometery, absorbance value was measured at 267nm. In first derivative spectrophotometry amplitudes were measured at 213nm. In second derivative spectrophotometry amplitudes were measured at 276nm. Calibration curves were linear between the concentration range of 20-60μg/ml, 20-60μg/ml and 40-80μg/ml respectively. The % RSD value is less than 2% and the recovery were near 100% for all methods. This method has been validated for linearity, accuracy and precision and found to be rapid, precise, accurate and economical and can be applied for routine estimation of sitagliptine in solid dosage form. The validation of method was carried out utilizing ICH-guidelines.

Derivative Spectrophotometric Methods for the Determination of Bendamustine Hydrochloride.

Bendamustine hydrochloride is used to treat chronic lymphocytic leukemia. It kills the existing cancer cells and limits the growth of new cancer cells. Three simple, rapid and sensitive spectrophotometric methods were developed for the determination of Bendamustine hydrochloride in phosphate buffer (pH 8.0) (Method A) and boric buffer (pH 9.0) (Method B). Method C is a difference spectroscopy technique in which the amplitude was chosen for the analytical calculations. Bendamustine hydrochloride obeys Beer-Lambert’s law over the concentration range 1-40 μg/ml, 0.1-40 μg/ml and 5- 40 μg/ml with regression equations y = 0.003x + 0.001(r² = 0.998) y = 0.0027x + 0.0005 (r² = 0.999), and y = 0.0034x + 0.006 (r² = 0.994) for Method A, B and C respectively. The methods were validated as per ICH guidelines and can be applied for the determination of Bendamustine hydrochloride in pharmaceutical formulations.