摘要
建立了测定大鼠血浆中福斯克林的液相色谱-串联质谱法(LC-MS/MS)。血浆样品经液-液萃取后,以V(甲醇):V(10mmol/L醋酸铵):V(甲酸)=75:25:0.1为流动相,用Hypersil ODS柱分离,流速0.8mL/min(柱后分流50%),通过电喷雾离子化四极杆串联质谱,以多反应监测方式(MRM)检测。用于定量分析的离子分别为m/z428/375(福斯克林)和m/z494/369(格列本脲,内标)。福斯克林血浆浓度测定方法的线性范围为0.8~800μg/L;日内、日间精密度(RSD)均小于10%;准确度(RE)小于±9%。每个样品测试时间4.5min。应用此法测试了大鼠口服或静注福斯克林后的血药浓度。
A rapid, sensitive and specific high pertbrmanee liquid chromatography tandem mass spectrometric (LC-MS/MS) method was developed for the determination of forskolin in rat plasma. Forskolin and internal standard, glibenclamide, were extracted from rat plasma using liquid-liquid extraetion, then separated on a Hypersil ODS column( 150 mm ×4.6 mm i. d., with 5 μm particle size). The mobile phase consisted of methanol-10 mmol/L ammonium acetate-formic acid (75:25:0. 1) , at a flow-rate of 0.8 mL/min. An API 3000 tandem mass spectrometer equipped with electrospray ionization source was used as detector and was operated in the positive ion mode. Multiple reaetions monitoring (MRM) mode with the transitions of m/z 428/375 and m/z 493/369 was used to quantify forskolin and internal standard, respectively. A limit of quantifieation 0.8μg/L for forskolin was aehieved in rat plasma. The chromatographic run time was 4.5 min and the weighted ( 1/x^2 ) calibration curve was linear in the range from 0.8 to 800 bLg/L for forskolin. The intra and inter-day precision was measured to be below 10%. The relative error was within± 9%. From the intra- and inter-day precision and accuracy, the present method satisfies the accepted criteria for bioanalytical method validation. The method is shown to be suitable for investigation of forskolin pharmaeokinetics.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2009年第3期399-402,共4页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No.30672508)
北京市自然科学基金(No.7072061)资助项目
关键词
福斯克林
液相色谱-串联质谱法
药代动力学
Forskolin, liquid chromatography tandem mass spectrometry, pharmacokinetics