HPLC-ECD法测定小鼠血浆中异丙肾上腺素浓度  

HPLC-ECD determination of isoproterenol concentration in mouse plasma

作　　者：刘亦伟[1] 王长连[1] 黄品芳[1] 

机构地区：[1]福建医科大学附属第一医院,福州350005

出　　处：《药物分析杂志》2011年第6期1098-1101,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的：建立高效液相色谱-电化学法测定小鼠血浆中异丙肾上腺素浓度,为研究其在小鼠体内药代动力学过程提供检测手段。方法：采用SymmetryShield C18柱（4.6 mm×250 mm,5.0μm）,流动相为含0.05 mol.L-1柠檬酸,0.05 mol.L-1无水乙酸钠,0.3 mmol.L-1EDTA-Na2,1.0 mmol.L-1IPR-B8离子对试剂,0.06 mmol.L-1二正丁胺,1.6%甲醇水溶液。流速：0.9 mL.min-1,柱温25℃。以3,4-二羟基苄胺为内标;用电化学检测器测定,检测电压：700 mV。测定小鼠皮下注射异丙肾上腺素（0.75 mg.kg-1）后不同时间的血浆药物浓度,用3P97软件拟合计算相关药动学参数。结果：IP在浓度范围为0.5~294.0 ng.mL-1内,线性关系良好（r=0.9998,n=7）。平均提取回收率为85.8%,平均回收率为100.9%,日内及日间RSD均小于3.9%（n=5）。最低检测限为0.08 ng.mL-1（S/N≥3）。相关药动学参数为AUC0-t=2424.76 min.ng.mL-1,Vc=2774 mL.kg-1,Cl=0.309 mL.g-1.min-1,Ka=（0.9817±0.174）min-1,Lag Time=（0.3076±0.0375）min。结论：本法准确、快速、稳定、灵敏度高,可用于生物样品中异丙肾上腺素浓度测定。Objective：To develop an HPLC-ECD method for determination of isoproterenol（IP） concentration in plasma.Methods：IP can be separated on SymmetryShield C18（4.6 mm×250 mm,5.0 μm）column,the mobile phase was consisted of 0.05 mol·L-1citric acid monohydrate,0.05 mol·L-1sodium acetate anhydrous,0.3 mmol·L-1EDTA-Na2,1.0 mmol·L-1IPR-B8,0.06 mmol·L-1 dibutylamine and 1.6% Methanol,Flow rate was 0.9 mL·min-1,column temperature was 25 ℃.The electrochemical detector was set at 700 mV,and dihydroxybenzy-lamine（DHBA）was used as internal standard.IP concentration in mice plasma were determined after sc.administration（0.75 mg·kg-1）,the data were processed with 3P97 pharmacokinetic program.Results：The isoproterenol was linear over the range 0.5-294.0 ng·mL-1,the correlation coefficient was 0.9998（n=7）.The average extraction recovery was 85.8%,the average recovery was 100.9%,RSD of intra-day and inter-day were less than 3.9%（n=5）.The detection limit was 0.08 ng·mL-1（S/N≥3）.The main pharmacokinetic parameters were estimated to be as follows：AUC0-t=2424.76 min·ng·mL-1,Vc=2774 mL·kg-1,Cl=0.309 mL·g-1·min-1,Ka=（0.9817±0.174） min-1,Lag Time=（0.3076±0.0375） min.Conclusion：The method is accurate,rapid and high sensitivity,it was suitable for the determination of isoproterenol in biological sample.

关 键 词：异丙肾上腺素 高效液相色谱-电化学法 血药浓度 

分 类 号：R917[医药卫生—药物分析学]