Development and Validation of GC-MS and HPLC Methods for the Determination of Simvastatin in Tablets and Human Urine

Abstract:

The present work reports rapid, sensitive and specific methods for determination of simvastatin in tablets and human urine by gas chromatography with mass spectrometry (GC-MS) and high-performance liquid chromatography with UV detection (HPLC-UV). The GC-MS method involved the separation of simvastatin without derivatization prior to analysis using 5% Phenyl Polysilphenylene-siloxane (TR-5MS) column with temperature programming. The EI mass spectrum of simvastatin was characterized by [M]⁺ at 418 and a base peak at m/z 159. In the HPLC method, the chromatographic behavior of simvastatin in micellar and aqueous-organic mobile phases using a short C8 column was investigated and simvastatin was detected at 240 nm. The methods were validated according to ICH guideline. The GC-MS and HPLC methods were successfully applied for the determination of simvastatin in tablets either alone or co-formulated with ezetimibe. Furthermore, the proposed methods were applied for the determination of simvastatin in human urine as a preclinical toxicology evaluation with no interfering peaks were observed from urine matrix.

Key words:

• Simvastatin
• GC-MS
• HPLC
• tablets
• urine