Palnati Narmada

To estimate the level of Phenylhydrazine, a potential genotoxic impurity in Ondansetron Hydrochloride API, a new simple, sensitive and accurate method was developed using Liquid Chromatographic Mass Spectrometry (LC-MS/MS). The chromatographic separation was achieved on Inert Sustain Swift C18, 5µ (150 x 4.6) mm column with gradient programme and elution was monitored by mass spectrometer in Multiple Reaction Monitoring mode using electrospray ionization. The LOD and LOQ values found to be 5 ppm and 15 ppm for the impurity with respect to the test concentration 2 mg/ml. The method was linear (r2>0.99), precise (RSD<2%), accurate and well within acceptable ICH limits.

A new, simple, accurate and sensitive method was developed for the quantification of two potential genotoxic impurities 1-(2-methyl-5-nitro-phenyl)guanidine nitrate and  N-(2-methyl-5-nitro-phenyl)-4-(3-pyridyl)pyrimidin-2-amine at low level (2 ppm) in Imatinib using liquid chromatographic mass spectrometry. The chromatographic separation was achieved on Kromasil 100-3.5-C18 (150 x 2.1) mm column with gradient programme and elution was monitored by mass spectrometer in selective ion monitoring mode using electrospray ionization. The LOD and LOQ values found to be 0.2 ppm and 0.6 ppm for both the impurities with respect to the test concentration 5 mg/ml. The method was linear (r2>0.99), precise (RSD

A specific and sensitive liquid chromatography-electrospray ionization tandem mass spectrometry method was developed for the determination of zolmitriptan in human plasma. Zolmitriptan and the internal standard (IS) rizatriptan were extracted by liquid–liquid extraction and were separated on a sunfire C18 column (100 x 2.1mm and 3.5µm) with isocratic elution of mobile phase consisting of 10mM ammonium formate containing 0.1% formic acid and acetonitrile. Electrospray ionization in multiple reaction monitoring mode was used to monitor the parent and the daughter ions of the analyte and the internal standard. The response is linear over a range of 0.5 to 100.0 ng/ml concentration with a correlation coefficient (r2) greater than 0.99 and an extraction efficiency of about 95%. The validated method can be applied to pharmacokinetic, toxicokinetic and bioequivalence studies.