A validated chiral LC method for the determination of Zolmitriptan and its potential impurities

作者：Srinivasu MK^*; Rao BM; Sridhar G; Kumar PR; Chandrasekhar KB; Islam A

来源：Journal of Pharmaceutical and Biomedical Analysis, 2005, 37(3): 453-460.

DOI：10.1016/j.jpba.2004.10.021

• zolmitriptan
• chiral HPLC
• Chiralpak AD-H
• validation
• zolmitriptan impurities
• solution and mobile phase stability

A new, accurate and reliable chiral HPLC method was developed for the determination of Zolmitriptan, (4S)-4-[[3-[2-(dimethylamino)ethyl]-1H-indol-5-yl] methyl]-2-oxazolidinone an antimigraine agent and its potential impurities namely (4R)-4-[[3-[2-(dimethylamino)ethyl]-1H-indol-5-yl] methyl]-2-oxazolidinone [(R)-enantiomer] and (4S)-4-(4-aminobenzyl)-2-oxazolidinone (Imp-1) in pharmaceutical formulations and in bulk drugs. HPLC separation was carried out by normal phase chromatography with a mobile phase composed of hexane:isopropanol:methanol:diethylamine in the ratio (75:10:15:0.1, v/v/v/v) pumped at a flow rate of 1.0 ml/min on a Chiralpak AD-H column. Zolmitriptan and its potential impurities were baseline resolved in the optimized method. The presence of diethylamine in the mobile phase has played a key role in achieving chromatographic resolution between the enantiomers and also in enhancing chromatographic efficiency. The developed method was also found to be selective under exposed conditions UV light and 60 degrees C. The developed method was completely validated and proved to be robust. The values of the limit of detection (LOD) and limit of quantification (LOQ) of (R)-enantiomer and Imp-1 were 100, 250 ng/ml and 30, 1000 ng/ml, respectively, for 10 mu l injection volume. The validated method yielded good results regarding selectivity. linearity, precision, accuracy and ruggedness. Zolmitriptan sample solution and mobile phase are found to be stable for at least 24 h. The proposed method was found to be suitable and accurate for the quantitative determination of Zoltmitriptan and its impurities namely (R)-enantiomer and Imp-1 in bulk drugs and commercial formulations.

• 出版日期2005-3-9