Department of Chemistry, School of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2012 May 1;895-896:154-61. doi: 10.1016/j.jchromb.2012.03.036. Epub 2012 Apr 1.
A simple and sensitive method for simultaneous determination of seven active constituents, jatrorrhizine, berberine, coptisine, palmatine, evodiamine, rutacarpine and paeoniflorin, from a Chinese medicine Wuji Pill in rat plasma was developed based on a liquid chromatography and tandem mass spectrometry method. The separation of these seven compounds was carried out on a Shiseido CAPCELL PAK C(18) column using a mobile phase consisting of acetonitrile (containing 0.1% formic acid and water (containing 0.1% formic acid and 10 mmol/L ammonium acetate) and carbamazepine as an internal standard. Electrospray ionization in positive-ion mode and multiple reaction monitoring was used to identify and quantitate active components. All calibration curves gave good linearity (r>0.993) over the concentration range from 0.42-208.0 ng/mL to 4.18-418.0 ng/mL for all components. The precision of the in vivo study was evaluated by intra- and inter-day assays and the percentages of relative standard deviation were all within 15%. The method was successfully applied to pharmacokinetic study of all six alkaloids and one monoterpene in rat plasma after oral administration of the Wuji Pill.
建立了一种基于液相色谱-串联质谱法同时测定大鼠血浆中六种生物碱和一种单萜类化合物吴茱萸次碱的含量。采用 Shiseido CAPCELL PAK C18 柱，以乙腈（含 0.1%甲酸）-水（含 0.1%甲酸和 10mmol/L 乙酸铵）为流动相，卡马西平为内标，在正离子模式下采用电喷雾电离，多反应监测进行检测。所有成分在 0.42-208.0ng/mL 至 4.18-418.0ng/mL 浓度范围内均具有良好的线性（r>0.993）。日内和日间精密度的测定结果表明相对标准偏差均在 15%以内。该方法成功应用于大鼠灌胃吴茱萸丸后六种生物碱和一种单萜类化合物的药代动力学研究。
