title: An efficient separation and method development for the quantifying of two basic impurities of Nicergoline by reversed-phase high performance liquid chromatography using ion-pairing counter ions.
abstract: A quantification method was developed for the two basic impurities, one of which is also a metabolite, of Nicergoline (NIC), by using reversed-phase high performance liquid chromatography (RP-HPLC) and diode array detector (DAD). One of these compounds,10-methoxy-6-methylergoline-8beta-methanol-5-bromo-3-pyridinecarboxylate (1-DN) is the metabolite as well as the impurity whereas, the other 10-methoxy-1,6-dimethylergoline-8beta-methanol-5-chloro-3-pyridinecarboxylate (5-CN) is only an impurity. The chromatographic column was Phenomenex, Luna, 5 microm, C18 (2), 250 mm x 4.6 mm. Mobile phase was 0.1 M ammonium acetate (NH4Ac) solution containing 4 mM 1-octanesulfonicacid sodium salt (OSASS) and 6 mM tetrabutylammonium hydrogen sulphate (TBAHS) (pH: 5.9)/acetonitrile (ACN) (62:38) for 1-DN and (64:36) for 5-CN. Flow rate was 1.0 mL min-1. The diode array detector was operated at 285 nm, band width: 4 nm. Linearity was obtained in the concentration range of 0.032 x 10-5 to 3.828 x 10-5 M, y = 116.88x + 0.2773 (r2 = 0.99989); the limit of detection (LOD) and limit of quantification (LOQ) were determined as 0.012 x 10-5 and 0.041 x 10-5 M for 1-DN, respectively. Linearity was obtained in the concentration range of 0.034 x 10-5 to 4.092 x 10-5 M, y = 104.24x + 0.7486 (r2 = 0.99996); (LOD) and (LOQ) were determined as 0.014 x 10-5 and 0.046 x 10-5 M for 5-CN, respectively. The recovery was 100.65% for 1-DN and 100.32% for 5-CN. The amount of 1-DN in 30 mg NIC was found as 209.65 microg (0.70%) and the amount of 5-CN in 30 mg NIC was found as 27.62 microg (0.09%).
authors.affiliation: Marmara University, Faculty of Pharmacy, Department of Analytical Chemistry, Haydarpasa, 34668 Istanbul, Uskudar, Turkey. gyalcin@marmara.edu.tr
authors.forename: Güler
authors.initials: G
authors.lastname: Yalçin
authors.forename: Nüray
authors.initials: N
authors.lastname: Yüktaş
mesh_terms: D017738:Alkanesulfonic Acids / Q000737:chemistry; D000837:Anion Exchange Resins / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004340:Drug Contamination / Q000517:prevention & control; D009530:Nicergoline / Q000032:analysis*; D000644:Quaternary Ammonium Compounds / Q000737:chemistry; D015203:Reproducibility of Results; D014665:Vasodilator Agents / Q000032:analysis
chemical_list: D017738:Alkanesulfonic Acids; D000837:Anion Exchange Resins; D000644:Quaternary Ammonium Compounds; D014665:Vasodilator Agents; C009405:tetrabutylammonium; C042005:1-octanesulfonic acid; D009530:Nicergoline