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机构地区:[1]上海交通大学附属第一人民医院,上海200080 [2]复旦大学药学院,上海200032
出 处:《中国医院药学杂志》2004年第9期533-534,共2页Chinese Journal of Hospital Pharmacy
摘 要:目的 :建立人血浆中吗氯贝胺的反相高效液相色谱检测方法。方法 :血浆样品在碱性条件下 (pH11.0 )用二氯甲烷提取处理。色谱柱为 μ BondapakTM C18(3.9mm× 15 0mm ,10 μm) ,柱温37.0℃ ,流动相为乙腈 0 .0 6 7mol·L-1磷酸二氢钾溶液 (1∶5 ,pH2 .6 ) ,流速 1.0mL·min-1,内标为甲氧氯普胺 ,检测波长为 2 4 0nm。结果 :吗氯贝胺在 4 0~ 4 0 0 0 μg·L-1范围内线性关系良好 (r=0 .9999,n =8) ,血浆中最小检测浓度为 10 μg·L-1(S/N =3) ,提取回收率为 96 .4 8%~ 10 0 .38% ,方法回收率在 99.39%~ 10 3.0 7%之间 ,日内RSD≤ 8.14 % ,日间RSD≤ 6 .2 5 %。结论 :该方法快速、准确、灵敏度高、专一性强 ,可用于吗氯贝胺血浆浓度监测和药动学及生物利用度研究。OBJECTIVE To develop a reversed-phase HPLC method for the determination of moclobemide in human plasma. METHODS Moclobemide and internal standard (metoclopramide) were extracted from basified plasma (pH _11.0) with dichloromethane and separated on μ-Bondapak __TM C _18 column with a mobile phase consisting of acetonitrile and _0.067 mol·L_-1 potassium phosphate buffer solution (1∶5, adjusted to pH _2.6 with dilute hydrochloric acid ). The column temperature was maintained at _37.0 ℃. The eluent was pumped at a flow-rate of _1.0 mL·min_-1. The detective wavelength was 240 nm. RESULTS The linearity was excellent over the range of 40-_4 000 μg·L_-1 (r=_0.999 9,n=8). The limit of detection was 10μg·L_-1 at a sign to noise ratio of 3/1. The extractive recoveries were from _96.48%-_100.38%. The methodological recoveries ranged from _99.39%-_103.07%. The within-day and between-days relative standard deviations (RSD) were _8.14% and _6.25%, respectively. CONCLUSION The elaborated method is rapid, sensitive, precise and selective, and can be used in measurement of moclobemide in plasma for therapeutic drug monitoring and pharmacokinetic studies.
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