Abstract

APPLICATION OF CENTRAL COMPOSITE DESIGN IN DEVELOPMENT OF VALIDATED STABILITY INDICATING HPTLC METHOD FOR DETERMINATION OF LANSOPRAZOLE AND DOMPERIDONE IN COMBINED DOSAGE FORM

A.G. Barsagade*, R.B. Kakde and S. R. Karmankar

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Abstract

The objective of current study was to develop a validated, specific stability indicating normal-phase high performance thin layer chromatographic method for simultaneous estimation of lansoprazole and domperidone in their combined dosage form. The forced degradation studies were performed on pure lansoprazole and domperidone and also on their combined dosage form using acid, base, neutral, oxidation, thermal and photo stress to show the stability indicating capability of the developed method. Significant degradation products were observed in acidic, basic, neutral and oxidation stress. No degradation products were obtained after photo and thermal stress condition. The chromatographic method was optimized using samples generated in forced degradation studies. Good separation between the peaks corresponding to the active pharmaceutical ingredients, lansoprazole and domperidone, and degradation product from the analyte were achieved on silica gel 60F254 TLC plate using toluene: methanol 8:2 (v/v) as mobile phase. Densitometric quantification was performed at 295 nm by reflectance scanning. The RF value of domperidone and lansoprazole were 0.34 ± 0.03 and 0.50 ± 0.03 respectively. As a pre validation part, robustness test was performed by applying a central composite design (CCD) to study the effect of critical factors on the method performance. Validation of the developed method was conducted as per ICH requirements. Response were a linear function of concentration of lansoprazole over the range 375–3000 ng/band by peak area with correlation coefficient 0.99693 and domperidone over the range 250–2000 ng/band by peak area with correlation coefficient 0.99372. The limit of detection of lansoprazole was 1.70 ng/band for peak area and the limit of detection of domperidone was 4.06 ng/band for peak area. Results from analysis of a commercial tablet formulation were 100.62 ± 0.0357 % and 100.00 ± 0.0388 % by peak area for lansoprazole and domperidone respectively. Recoveries were 100.06 ± 0.4690 % and 99.66 ± 0.2482 % by peak area for lansoprazole and domperidone respectively. The developed HPTLC method was found to suitable to check the quality of lansoprazole and domperidone combined dosage form.

Keywords: HPTLC, lansoprazole, domperidone, degradation products, validation, central composite design.