Affiliation:
1. 1Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, P.O. Box 35516, Mansoura, Egypt
2. 2Department of Pharmaceutical Chemistry, Faculty of Pharmacy, King Abdulaziz University, P.O. Box 80260, Jeddah 21589, Kingdom of Saudi Arabia
Abstract
AbstractA simple and sensitive liquid chromatography-mass spectrometric (LC-MS) method has been developed and validated for the simultaneous determination of ezetimibe (EZE), atorvastatin calcium (ATO), and simvastatin (SMV) in combined dosage forms and human plasma. Successful separation of the studied drugs was achieved on a Zorbax Eclipse Plus C18 column (3.0 × 150 mm, 5 µm) using a mobile phase consisting of acetonitrile and 0.1% formic acid in water (65:35, v/v) at a flow rate of 0.5 mL min−1. Total run time was 9.3 min and diclofenac sodium was used as internal standard (IS). Positive selected ion monitoring (SIM) mode was applied where, the monitored ions were those at m/z values of 392.1, 559.3, 296.0, and 441.4 corresponding to EZE, ATO, IS, and SMV, respectively. The method was fully validated according to the ICH guidelines. The intraday and interday precision showed relative SD values not more than 1.77 and 1.99%; respectively. The limits of detection (LOD) were 0.25, 0.25, and 0.75 ng mL−1 while the limits of quantification (LOQ) were 1.25, 0.75, and 2.5 ng mL−1 for EZE, ATO, and SMV, respectively. The developed method was applied on two types of combined tablets concerning drug assay with mean percent recoveries within acceptable range. The method has been extended to the determination of the studied drugs in human plasma where, a solid phase extraction method was optimized for their extraction with percent recovery not less than 97%.