摘要
目的:用高效液相色谱-质谱联用方法同时测定大鼠血浆中普萘洛尔及其代谢物4-羟普萘洛尔、N-去异丙基普萘洛尔的浓度。方法:大鼠血浆用乙醚萃取法处理后,采用 LC/MS/MS 方法,测定大鼠血浆中普萘洛尔及其代谢物4-羟普萘洛尔、N-去异丙基普萘洛尔的浓度。HPLC 条件:大连依利特 Hypersil BDS C_(18)柱(2.1 mm×50 mm,3μm),流动相:水(含0.1%甲酸)-乙腈(39:61,v/v),柱温:12℃,流速:200 μL·min^(-1),进样量:10 μL;质谱检测参数为电喷雾电离源(ESI);喷雾电压:3500 V;碰撞压力:0.1333 Pa;源内碰撞诱导电压:普萘洛尔,10 V;4-羟普萘洛尔,15 V;N-去异丙基普萘洛尔,15 V;扫描时间:0.3 s;检测离子:普萘洛尔 m/z 260[M+H]^+;4-羟普萘洛尔 m/z 276[M+H]^+;N-去异丙基普萘洛尔218[M+H]^+。结果:普萘洛尔线性范围2—1000 ng·mL^(-1),最低定量限为2 ng·mL^(-1)。4-羟普萘洛尔和 N-去异丙基普萘洛尔的线性范围1～200 ng·mL^(-1),最低定量限为1 ng·mL^(-1)。普萘洛尔的萃取回收率在90%以上,4-羟普萘洛尔和 N-去异丙基普萘洛尔的萃取回收率均为50%以上,日内、日间 RSD 皆小于15%。结论:适用于测定大鼠血浆中普萘洛尔及其代谢物4-羟普萘洛尔、N-去异丙基普萘洛尔的浓度及药动学的研究。
Objective： To establish an LC/MS/MS method for the determination of propranolol and its metabolites 4 - hydroxypropranolol and N - desisopropylpropranolol in rat plasma. Methods： HPLC ： Use Hypersil BDS C18 column （ 3 μm,2. 1 mm × 50 mm） ; The mobile phase consisting of water - acetonitrile （ 39：61, v/v）, a flow rate of 200 μL · min^ - 1, injection volume 10 μL. MS ： m/z 260 （ propranolol）, m/z 276 （ 4 - hydroxypropranolol ）, m/z 218 （ N - desisopropylpropranoM） ; Polarity ： Positive ; Ionization source ： ESI ; Spray voltage ：3500 V ; Collision pressure ：0. 1333 Pa;Source CID： propranolol—10 V, 4 -hydroxypropranolol and N- desisopropylpropranolol—15 V. The plasma samples were extracted with ether. Results ：The linear range of propranolol was 2 - 1000 ng · mL^-1 and LOQ of detection was 2 ng · mL^- 1. The linear range of 4 - hydroxypropranolol and N - desisopropylpropranolol was 1 - 200 ng · mL^-1 and LOQ was 1 ng · mL^-1. Propranolol extraction recovery rates were more than 90% ,4 - hydroxypropranolol and N- desisopropylpropranolol extraction recovery rates were more than 50% ;Intra- day RSD and inter- day RSD were less than 15%. Conclusion： This method is found to be sensitive,fast, and accurate ,which it can be used for pharmacokinetic studies of propranolol in rat plasma.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2005年第10期1203-1206,共4页
Chinese Journal of Pharmaceutical Analysis
