Song M, Hang T J, Zhang Zh X, Du R, Chen J
Department of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing 210009, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Dec 5;827(2):205-9. doi: 10.1016/j.jchromb.2005.09.014. Epub 2005 Sep 23.
A sensitive and selective LC-MS-MS method has been developed and validated for the determination of cryptotanshinone (CTS) and its active metabolite tanshinone II A (TS II A) in rat plasma using fenofibrate (FOFB) as internal standard. Liquid-liquid extraction was used for sample preparation. Chromatographic separation was achieved on a Waters symmetry ODS column using methanol and water (85:15) as mobile phase delivered at 1.0 mL/min. LC-MS-MS analysis was carried out on a Finnigan LC-TSQ Quantum mass spectrometer using atmospheric pressure chemical ionization (APCI) and positive multiple reaction monitoring. Ions monitored were m/z 297.0--> 251.0 for CTS, m/z 295.0--> 249.0 for TS II A, and m/z 361.1--> 233.0 for FOFB with argon at a pressure of 0.2 Pa and collision energy of 25 eV for collision-induced dissociation (CID). The assay was linear over the range 0.1-20 ng/mL for CTS and 0.2-15 ng/mL for TS II A. The average recoveries of CTS and TS II A from rat plasma were 93.7 and 94.7%, respectively. The established method has been applied in a pharmacokinetic study of CTS in rats.
已开发并验证了一种灵敏且具选择性的液相色谱-串联质谱法，以非诺贝特（FOFB）为内标，用于测定大鼠血浆中的隐丹参酮（CTS）及其活性代谢物丹参酮II A（TS II A）。采用液-液萃取法进行样品制备。在Waters symmetry ODS柱上进行色谱分离，以甲醇和水（85:15）为流动相，流速为1.0 mL/min。在Finnigan LC-TSQ Quantum质谱仪上进行液相色谱-串联质谱分析，采用大气压化学电离（APCI）和正离子多反应监测模式。监测的离子为：CTS的m/z 297.0→251.0、TS II A的m/z 295.0→249.0以及FOFB的m/z 361.1→233.0，氩气压力为0.2 Pa，碰撞能量为25 eV用于碰撞诱导解离（CID）。该测定法在CTS浓度范围为0.1 - 20 ng/mL、TS II A浓度范围为0.2 - 15 ng/mL时呈线性。CTS和TS II A从大鼠血浆中的平均回收率分别为93.7%和94.7%。所建立的方法已应用于CTS在大鼠体内的药代动力学研究。
