School of Pharmacy, Second Military Medical University, Shanghai 200433, PR China.
J Pharm Biomed Anal. 2010 May 1;52(1):155-9. doi: 10.1016/j.jpba.2009.12.013. Epub 2009 Dec 21.
An ultra-performance liquid chromatography/quadrupole time-of-flight mass spectrometry method was established to detect as many constituents in rat biological fluids as possible after oral administration of Fufang Danshen tablets (FDTs). A C18 column (1.8microm particle size) was adopted to separate the samples, and mass spectra were acquired in both negative and positive modes. First, the fingerprints of FDTs were established, resulting in 43 components being detected within 25min. Among these compounds, 37 were tentatively identified by comparing the retention times and mass spectral data with those of reference standards and the reference literature; the other 6 components were tentatively assigned solely based on the MS data. In vivo, 14 components and 8 metabolites of FDT were observed in plasma, and 12 components of FDT were detected in urine. Tanshinaldehyde, danshexinkun B, a glycine conjugate of danshensu and a methylated conjugate of danshexinkun B were newly detected in rat biological fluids. This study developed a high-speed and sensitive method that was successfully utilized for screening the active ingredients of a Chinese medical formula and provided helpful chemical information for further pharmacology and active mechanism research on Chinese medicine.
建立了超高效液相色谱/四极杆飞行时间质谱法,以尽可能多地检测口服复方丹参片(FDTs)后大鼠生物体液中的成分。采用 C18 柱(1.8μm 粒径)分离样品,并在正负模式下采集质谱。首先建立了 FDTs 的指纹图谱,在 25min 内检测到 43 个成分。其中,37 个化合物通过与对照品和参考文献中的保留时间和质谱数据进行比较进行了初步鉴定;其余 6 个成分仅根据 MS 数据进行了初步归属。在体内,观察到血浆中 FDT 的 14 种成分和 8 种代谢物,尿液中检测到 FDT 的 12 种成分。在大鼠生物体液中首次检测到丹参醛、丹参新醌 B、丹参酸甘氨酸缀合物和丹参新醌 B 的甲基化缀合物。本研究开发了一种高速灵敏的方法,成功用于筛选中药配方的活性成分,并为进一步的中药药理学和作用机制研究提供了有价值的化学信息。