A stability indicating LC method for zolmitriptan.
A gradient, reversed-phase liquid chromatographic (RP-LC) assay method was developed for the quantitative determination of zolmitriptan, used to treat severe migraine headaches. The developed method is also applicable for the related substances determination in bulk drugs. The chromatographic separation was achieved on a Waters X Terra RP18, 250 mm x 4.6 mm, 5 microm column. The gradient LC method employs solutions A and B as mobile phase. The solution A contains a mixture of phosphate buffer pH 9.85:methanol:acetonitrile (70:20:10, v/v/v) and solution B contains a mixture of phosphate buffer, pH 9.85:acetonitrile (30:70). The flow rate was 1.0 ml/min and the detection wavelength was 225 nm. In the developed HPLC method, the resolution between zolmitriptan and its potential impurities, namely Imp-1, Imp-2 and Imp-3 was found to be greater than 3. The drug was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. Considerable degradation was found to occur in alkaline medium and oxidative stress conditions. Degradation product formed during base hydrolysis was found to be Imp-3. The stress samples were assayed against a qualified reference standard and the mass balance was found close to 99.5%. The developed RP-LC method was validated with respect to linearity, accuracy, precision and robustness.
Rao
B Mallikarjuna
BM
Analytical Research, Custom Pharmaceutical Services, Dr. Reddy's Laboratories, Hyderabad 500049, India. bmrao@drreddys.com
Srinivasu
M K
MK
Sridhar
G
G
Kumar
P Rajender
PR
Chandrasekhar
K B
KB
Islam
Aminul
A
D000097:Acetonitriles / Q000737:chemistry; D002021:Buffers; D002138:Calibration; D002626:Chemistry, Pharmaceutical / Q000379:methods*; D002845:Chromatography; D002851:Chromatography, High Pressure Liquid; D002853:Chromatography, Liquid / Q000379:methods*; D004345:Drug Industry / Q000379:methods*; D006863:Hydrogen-Ion Concentration; D006868:Hydrolysis; D008956:Models, Chemical; D023303:Oxazolidinones / Q000032:analysis* / Q000737:chemistry; D010100:Oxygen / Q000737:chemistry; D019999:Pharmaceutical Solutions / Q000032:analysis; D010782:Photolysis; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D017366:Serotonin Receptor Agonists / Q000032:analysis / Q000737:chemistry; D012995:Solubility; D014363:Tryptamines / Q000032:analysis* / Q000737:chemistry
D000097:Acetonitriles; D002021:Buffers; D023303:Oxazolidinones; D019999:Pharmaceutical Solutions; D017366:Serotonin Receptor Agonists; D014363:Tryptamines; C089750:zolmitriptan; D010100:Oxygen; C032159:acetonitrile