Department of Pharmacy, Changzheng Hospital, Second Military Medical University, No. 415 Fengyang Road, Shanghai 200003, PR China.
J Pharm Biomed Anal. 2010 Sep 5;52(5):741-6. doi: 10.1016/j.jpba.2010.02.003. Epub 2010 Feb 10.
A rapid sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for simultaneous determination of multiple bioactive lignan constituents of Wuzhi capsule in rat plasma. The extraction, separation, and analytical conditions were optimized. Five constituents of the Wuzhi capsule (schisandrin, schisandrol B, schisantherin A, schisanhenol, and deoxyshisandrin) were determined by the LC-MS/MS method. Liquid-liquid extraction with methyl tert-butyl ether was carried out using bifendate as the internal standard. The five bioactive constituents were separated on a Zorbax SB-C18 reserved-phase column (100 mm x 2.1 mm i.d., 3.5 microm) by isocratic elution using a mobile phase consisting of acetonitrile, methanol, and 0.1% aqueous formic acid (72:18:10, v/v/v) at a flow rate of 0.3 mL/min. The total run time was only 3.5 min. All analytes showed good linearity over a wide concentration range (r(2)>0.99) and their lower limit of quantification was 0.5 ng/mL. The average extraction recovery of the five analytes from rat plasma was more than 85%, and the intra-day and inter-day accuracy and precision of the assay were less than 15%. Our method was successfully used for pharmacokinetic study of the five components in the Wuzhi capsule.
建立了一种同时测定大鼠血浆中五酯胶囊中多种生物活性木质素成分的快速灵敏、选择性好的液相色谱-串联质谱（LC-MS/MS）方法。优化了提取、分离和分析条件。采用 LC-MS/MS 法测定五酯胶囊中的 5 种成分（五味子甲素、五味子乙素、五味子丙素、五味子醇甲和五味子醇乙）。以双飞蓟宾为内标，采用甲基叔丁基醚进行液液萃取。在 Zorbax SB-C18 保留柱（100mm×2.1mmid，3.5μm）上，采用乙腈、甲醇和 0.1%甲酸水溶液（72:18:10，v/v/v）作为流动相，以 0.3mL/min 的流速进行等度洗脱，分离 5 种生物活性成分。总运行时间仅为 3.5min。所有分析物在较宽的浓度范围内均表现出良好的线性（r²＞0.99），定量下限为 0.5ng/mL。5 种分析物从大鼠血浆中的平均提取回收率均大于 85%，日内和日间准确度和精密度均小于 15%。该方法成功用于五酯胶囊中 5 种成分的药代动力学研究。
