HPLC紫外检测法测定血浆甲磺酸瑞波西汀浓度  

Determination of Reboxetine Mesilate in Plasma by High Performance Liquid Chromatography with Ultraviolet Detection

作　　者：张军[1] 李文标[1] 郭桂欣[1] 翟屹民[1] 果伟[1] 王传跃[1] 

机构地区：[1]首都医科大学附属北京安定医院临床精神药理实验室

出　　处：《首都医科大学学报》2008年第4期431-435,共5页Journal of Capital Medical University

摘　　要：目的建立测定血浆甲磺酸瑞波西汀浓度的高效液相色谱检测法。方法以麦普替林为内标,取血浆样本1mL,用饱和Na2HPO4碱化后以重蒸乙醚5mL提取,再用0.2mol.L-1盐酸0.2mL反提取,80℃～100℃热水浴下氮气吹干盐酸层,用50μL流动相重组后进样。采用InertsilODS-3柱(GLSciense,5μm,4.6mm×150mm)进行分离。流动相为乙腈-50mmol/L磷酸钠缓冲液(pH=6)(40:60,v/v),流速为0.6mL.min-1,紫外检测波长210nm。结果瑞波西汀对内标的峰高比与血浆甲磺酸瑞波西汀浓度直线相关,相关系数r=0.9997,线性范围3.12～200ng.mL-1。甲磺酸瑞波西汀的最低检测限0.5ng,最低检测浓度2ng.mL-1,提取回收率在82.50%～86.08%之间,批内和批间RSD分别为2.02%～5.33%和3.83%～8.50%。结论本法具有较高的灵敏度、精密度和特异性,适用于甲磺酸瑞波西汀的药代动力学和治疗药物监测的研究。Objective To develop a method for the determination of reboxetine mesilate in plasma by high performance liquid chromatography. Methods With maprotiline hydroehloride as the internal standard, 1 mL plasma sample was extracted with 5 mL distilled diethyl ether and re-extracted with 0.2 mol· L^-1 HCl 0.2 mL. The HCl phase was evaporated to dryness with N2 stream at 80℃ - 100℃ ,and the residues were dissolved with 50 μL mobile phase. The compounds were separated on an Inertsil ODS-3 column （GL Sciences, 5 μm, 4.6 mm × 150 mm）. The mobile phase was composed of aeetonitrile -50 mmol/L sodium phosphate（pH =6） （40 ： 60, v/v） and vacuum filtered with 0.45 μmol/L micro filtration film. The flow rate of mobile phase was 0.6 mL · min^-1. The UV detection wave length was 210 nm. Results The relationship of the peak height ratio of reboxetine mesilate to maprotiline vs. reboxetine mesilate concentration in plasma was linear within the range of 3.12 -200 ng · mL^-1, r = 0.999 7. The lowest detection limit was 0.5 ng and the lowest concentration detected was 2 ng· mL^-1. The extraction recovery of reboxetine mesilate was 82.50% - 86.08%. The within-and between-batch preeisions were 2.02% - 5.33% and 3.83% - 8.50%, respectively. Conclusion The method is sensitive, precise, reproducible and specific, and can be used in the pharmacological research and therapeutic monitoring of reboxetine mesilate.

关 键 词：甲磺酸瑞波西汀 血浆浓度 高效液相色谱 紫外检测法 

分 类 号：R971.4[医药卫生—药品] R971.1[医药卫生—药学]