【作者】 王平； 梁逸曾； 陈本美； 易伦朝； 周能； 袁大林；

【Author】 WANG Pinga, LIANG Yi-zenga,*, CHEN Ben-Meib, YI Lun-zhaoa, ZHOU Nenga, YUAN Da-lina aCollege of Chemistry and Chemical Engineering, Research Center of Modernization of Chinese Medicines, Central South University,Changsha 410083,P.R. China; bAnalytical Testing center of Xiangya medical School, Central South University,Changsha 410078,P.R. China

【机构】 中南大学中药现代化研究中心； 中南大学湘雅医学院分析测试中心；

【Abstract】 A sensitive liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) method had been developed and validated for rapid determination of amantadine in human plasma. Desloratadine was used as the internal standard (I.S.). 0.2mL of human plasma was alkalified with100μl of sodium hydroxide (3M) and extracted with 1mL of n-hexane containing 1% isopropanol (v/v) and 10% dichloromethane (v/v) by vortex-mixer for 3min. The mixture was centrifuged at 14000r/min for 5min. The supernatant was evaporated to dryness and dissolving in mobile phase, samples were separated using a Thermo Hypersil-HypurityC18 reversed-phase column(150mm×2.1mm i.d.,5μm). Mobile phase consisted of methanol-acetonitrile-20mM ammonium acetate (45:10:45,v/v/v) containing 1% acetic acid with a pH of 4.0. Amantadine and I.S. were measured by electrospray ion source in positive selective ion monitoring mode. The good linearity ranged from 3.9 to1000ng/ml and the limits of detection and quantification were about 3.9ng/ml. The extraction efficiencies were approximately 70% and recoveries of method ranged from 98.55% to 103.24%. The intra-day relative standard deviations (R.S.D.) were less than 8.43% and inter-day R.S.D. were below 10.59%. QC samples were stable when kept at room temperature for 12h,at –20°C for 30 days and after four freeze/thaw cycles.更多还原