Chen Chun-Yun, Qi Lian-Wen, Yi Ling, Li Ping, Wen Xiao-Dong
Key Laboratory of Modern Chinese Medicines, China Pharmaceutical University, Ministry of Education, Nanjing 210009, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2009 Jan 15;877(3):159-65. doi: 10.1016/j.jchromb.2008.11.043. Epub 2008 Dec 6.
A liquid chromatography-electrospray ionization-mass spectrometry method has been developed and validated for identification and quantification of four major bioactive saponins in rat plasma after oral administration of extraction of saponins from Flos Lonicerae, i.e., macranthoidin B, macranthoidin A, dipsacoside B, and macranthoside B. Plasma samples were extracted with solid-phase extraction, separated on a Shim-pack CLC-ODS column and detected by MS in negative selective ion monitoring mode. Calibration curves offered linear ranges of two orders of magnitude with r(2)>0.999. The method showed the low limit quantification of 7.72, 6.06, 7.16, and 1.43 ng/mL for macranthoidin B, macranthoidin A, dipsacoside B, and macranthoside B, respectively. The inter- and intra-CV precision (R.S.D.) were all within 10% and accuracy (% bias) ranged from -10 to 10%. The overall recovery was more than 70%. This developed method was subsequently successfully applied to pharmacokinetic profiles of the four saponins in rats. After oral administration of extraction of saponins in rats, the concentration-time course was found to be the double peaks of curve.
建立了一种液相色谱 - 电喷雾电离 - 质谱法,并对其进行了验证,用于在大鼠口服忍冬花皂苷提取物后,鉴定和定量大鼠血浆中的四种主要生物活性皂苷,即大花忍冬苷B、大花忍冬苷A、续断皂苷B和大花忍冬苷B。血浆样品采用固相萃取法提取,在Shim-pack CLC-ODS柱上分离,并在负选择性离子监测模式下通过质谱检测。校准曲线的线性范围为两个数量级,r(2)>0.999。该方法对大花忍冬苷B、大花忍冬苷A、续断皂苷B和大花忍冬苷B的定量下限分别为7.72、6.06、7.16和1.43 ng/mL。批间和批内变异系数(R.S.D.)均在10%以内,准确度(%偏差)范围为-10%至10%。总回收率超过70%。随后,该方法成功应用于大鼠体内四种皂苷的药代动力学研究。大鼠口服皂苷提取物后,发现浓度 - 时间曲线为双峰。