液相色谱-质谱联用法测定美金刚在人体中的血药浓度  

Determination of memantine in human plasma by LC-MS

作　　者：陈巧明[1] 黄贤君[2] 杨伟权[1] 

机构地区：[1]中山大学附属第一医院药学部,广东广州510080 [2]中山大学附属第一医院麻醉科,广东广州510080

出　　处：《中国医院药学杂志》2012年第19期1523-1526,共4页Chinese Journal of Hospital Pharmacy

摘　　要：目的:建立LC-MS法测定美金刚在血浆中的浓度。方法:血浆样品经过饱和碳酸氢钠溶液碱化后,用醋酸乙酯萃取用醋酸乙酯萃取;流动相:20 mmol·L-1醋酸铵水溶液(含0.05%醋酸)-甲醇(25∶75);色谱柱:Zorbax SB-C18(5μm,250 mm×4.6 mm ID,Agilent Technology)。质谱检测方式:选择性离子检测(SIM);离子极性:正离子(Positive);流动相为甲醇-10mmol·L-1(含0.5%甲酸)的醋酸铵水溶液(60∶40),流速为1.0mL·min-1,采用电喷雾离子化(ESI),以选择性离子检测(SIM)方式进行检测。结果:美金刚的线性范围在0.054 60～109.2 ng·mL-1,最低定量限为0.054 60 ng·mL-1,方法提取回收率为84.2%～84.9%,相对回收率为100.2%～103.6%,日内、日间RSD均<10%。结论:本方法准确,灵敏,重现性好,可用于美金刚血药浓度的检测及药动学的相关研究。OBJECTIVE To establish an HPLC-MS/MS method for the determination of memantine in human plasma.METHODS Donepezil was used as the internal standard.After alkalinization with saturated NaHCO3 solution,the plasma was extracted with 3 mL acetic ether and separated by LC on a reversed-phase C18 colunmn,with a mobile phase of 20 mmol·L-1 ammonium acetate buffer containing 0.05% acetic acid methanol（25∶75,v/v） at a flow rate of 1 mL·min-1.The column temperature was maintained at 25 ℃.Memantine was determined with ESI-MS.A quadrupole mass spectrometer equipped with an ESI source was set with a drying gas（N2） flow of 10 L·min-1,nebulizer pressure of 40 psig,drying gas temperature of 350 ℃,and the positive ion mode.The fragmentor voltage was 80 V.LC-ESI-MS was performed in the selected ion monitoring（SIM） mode using target ions at ＋ m/z 180.2 for memantine and ＋ m/z 380.2 for I.S..Endogenous substances didn＇t interfere the determination.RESULTS The linear calibration curves of memantine were in the ranges of 0.054 60-109.2 ng·mL-1,and the low determination limits were 0.054 60 ng·mL-1.The extraction recoveries of memantine were 84.2%-84.9 %,the relative recoveries of memantine were 100.2%-103.6%,and the intra-day and inter-day RSDs were less than 10%.CONCLUSION This method is sensitive and reproducible,and the results are reliable and accurate.

关 键 词：高效液相色谱-串联质谱法 美金刚 血药浓度 

分 类 号：R927[医药卫生—药学]