Teng Shi-Yong, Zhang Si-Xi, Niu Kai, Zhai Li-Jie, Wang Shi-Ji
Department of Anesthesiology, the First Hospital of Jilin University, Changchun, 130021, People's Republic of China.
Department of Pharmacy, the First Hospital of Jilin University, Changchun, 130021, People's Republic of China.
Biomed Chromatogr. 2015 Dec;29(12):1798-804. doi: 10.1002/bmc.3498. Epub 2015 May 29.
Bullatine A is a diterpenoid alkaloid of Xue-Shang-Yi-Zhi-Hao (Aconitum brachypodum), which is widely used in traditional Chinese medicine for the treatment of rheumatism and pain. The plasma levels of bullatine A were measured by a rapid and sensitive LC-MS/MS method. Samples were prepared using acetonitrile precipitation and the separation of bullatine A was achieved on a Capcell Pak MG-C18 column by isocratic elution using acetonitrile (phase A) and 0.1% formic acid (phase B, pH 4.0; A:B, 30:70, v/v) as the mobile phase at a flow rate of 0.5 mL/min. Detection was performed on a triple-quadrupole tandem mass spectrometer by multiple-reaction monitoring of the transitions at m/z 344.2 → 105.2 for bullatine A and m/z 256.2 → 167.1 for the internal standard. The linearity was found to be within the concentration range of 1.32-440 ng/mL with a lower limit of quantification of 1.32 ng/mL. Only 1.3 min was needed for an each analytical run. This method was successfully applied in the determination of the active component bullatine A in rat plasma after intramuscular administration of A. brachypodum injection.
布拉亭A是雪上一枝蒿（短柄乌头）中的一种二萜生物碱，在中国传统医学中广泛用于治疗风湿和疼痛。采用快速灵敏的液相色谱-串联质谱法（LC-MS/MS）测定布拉亭A的血浆水平。样品采用乙腈沉淀法制备，在Capcell Pak MG-C18柱上，以乙腈（A相）和0.1%甲酸（B相，pH 4.0；A:B，30:70，v/v）作为流动相，等度洗脱实现布拉亭A的分离，流速为0.5 mL/min。在三重四极杆串联质谱仪上进行检测，通过多反应监测布拉亭A的m/z 344.2 → 105.2和内标的m/z 256.2 → 十六十七点一的跃迁。线性范围为1.32 - 440 ng/mL，定量下限为1.32 ng/mL。每次分析运行仅需1.3分钟。该方法成功应用于大鼠肌肉注射短柄乌头注射液后血浆中活性成分布拉亭A的测定。
