高效液相色谱串联质谱法测定人血浆中美金刚浓度  被引量:5

Development of memantine in human plasma by liquid chromatography tandem mass spectrometry

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作  者:曲婷婷[1] 刘晓燕[1] 王本杰[2] 袁桂艳[2] 张蕊[2] 魏春敏[2] 郭瑞臣[2] 

机构地区:[1]山东大学药学院,山东济南250012 [2]山东大学齐鲁医院临床药理研究所,山东济南250012

出  处:《中国医院药学杂志》2009年第7期549-551,共3页Chinese Journal of Hospital Pharmacy

摘  要:目的:建立测定人血浆中美金刚浓度的高效液相色谱串联质谱法,以用于美金刚人体药动学研究。方法:Ultimate XB-C18柱(150mm×4.6mm,5μm)为色谱柱,甲醇-0.5%甲酸(70∶30)为流动相,流速为0.5mL·min-1;电喷雾电离正离子模式,选择性监测质荷比(M/Z)为180→163(美金刚)和152→135(金刚烷胺,内标);血浆样本经醋酸乙酯提取后进行分析。结果:血浆中美金刚质量浓度在0.2~100μg·L-1范围内线性关系良好,最低定量限达0.2μg·L-1;日内、日间精密度RSD小于7,血浆样本经冷冻和冻融后均稳定。结论:此方法灵敏、专一、快速、简便,适用于盐酸美金刚胶囊人体药动学研究。OBJECTIVE To validate a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the determination of memantine in human plasma. METHODS The analyte was separated on a Ultimate XB-C18 column(150 mm 4. 6 mm, 5 μm) with a mobile phase of methanol and water containing 0. 5% formic acid (70:30) at a flow rate of 0. 5mL·min^-1. The multiple reaction monitoring (MRM) mode was used for analyte quantification, and the precursor-to-prod- uct ion transition of m/z 180→163 (memantine) and 152→135 (amantadine, IS) were selected, respectively. The plasma sample was liquid-liquid extracted by ethyl acetate. RESULTS The weighted ( 1/x^2) calibration curve was linear in the 0.2 - 100. 0 μg·L^-1 range for memantine, and the low limit of quantification was 0. 2 μg·L^-1. The inter- and intra-day precisions (RSD) were 〈7. Plasma samples were stable under freezed and freeze-thaw conditions. CONCLUSION The developed LC/ MS/MS method was selective, sensitive and simple, and was successfully applied to the pharmacokinetic study of memantine after oral administration to Chinese healthy volunteers.

关 键 词:高效液相色谱串联质谱法 HPLC-MS/MS 美金刚 金刚烷胺 药动学 

分 类 号:R969[医药卫生—药理学]

 

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