Abstract
A novel, reversed-phase ultra-performance liquid chromatographic method was developed and validated for the determination of the assay and related substances of Lansoprazole (LAN) in bulk drug and capsule dosage forms. The related substances include degradation and process-related impurities. The method was developed using the Waters Acquity BEH C18 column and gradient program with mobile phase A as a pH 7.0 phosphate buffer and methanol in the ratio of 90: 10 (v/v), and mobile phase B as methanol and acetonitrile in the ratio of 50:50 (v/v). Lansoprazole and its impurities were monitored at 285 nm. Lansoprazole was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal, humidity, and photolytic degradation and found to degrade significantly under acid and oxidative stress conditions. The degradation products were well-resolved from the main peak and its impurities, proving the stability-indicating power of the method. The performance of the method was validated according to the present ICH guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision, ruggedness, and robustness.
Highlights
Initial method development started to separate all of the degradants of Lansoprazole, where the mobile phase pH was selected based on the pka value and the diluent pH was selected on the basic side by considering that Lansoprazole degrades in acidic conditions
The mobile phase was selected for development, with a buffer containing 20mM KH2PO4 and 8 ml of triethylamine in 1000 ml of Milli-Q water, and the pH was adjusted to 7.0 using orthophosphoric acid and methanol as organic solvents
Method development trials were initiated with an isocratic method and were able to separate all the known impurities related to Lansoprazole, but not the degradant peak formed during the acid degradation at RRT 1.05
Summary
Lansoprazole standard, Lansoprazole API, Imp 1, 2, 3, 4, and 5 standards with a purity of 99.8%, samples were supplied by Dr.Reddy’s laboratories Ltd, Hyderabad, India. The LC system of Waters Acquity UPLC with photodiode array detector was used for this study and chromatographic separation was achieved on the Acquity BEH-C18 (50 mm x 2.1 mm x 1.7 μm) column. The diluent used for the standard and sample preparation consisted of a pH 11.0 buffer and ethanol in the ratio of 80:20 (v/v)(7.6 grams of borax, 1 gram of edetate sodium in 1000 mL water, adjusted the pH to 11.0 with a diluted sodium hydroxide solution). A standard stock solution of LAN 400 μg/mL was prepared by dissolving the appropriate amount of drug in the diluent. Individual impurity stock solutions were prepared, diluted, and mixed to get 1.2 μg/mL, which was used for the method validation of LAN. An aliquot of 1.0 mL of this solution was diluted to 10mL with the diluent, yielding 40 μg/mL solution that was filtered through a 0.22 μm nylon membrane filter and used for the determination of the assay of LAN
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