Tan Guangguo, Zhu Zhenyu, Jing Jing, Lv Lei, Lou Ziyang, Zhang Guoqing, Chai Yifeng
Department of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, Shanghai 200433, People's Republic of China.
Biomed Chromatogr. 2011 Aug;25(8):913-24. doi: 10.1002/bmc.1544. Epub 2010 Nov 5.
A high-performance liquid chromatography with diode-array detection coupled to time-of-flight mass spectrometry (HPLC/DAD/TOFMS) method was established to clarify the chemical composition of Sini decoction (SND) and rat plasma after oral administration of SND. With dynamic adjustment of fragmentor voltage in TOFMS, an efficient transmission of the ions was achieved to obtain the best sensitivity for providing the molecular formula for each analyte and abundant fragment ions for structural information. By accurate mass measurements within 5 ppm error for each molecular ion and subsequent fragment ions, 53 compounds including diterpenoid alkaloids, flavonoids, triterpenoids and gingerol-related compounds were identified in SND. Major compounds identified from SND were further assigned in the three individual herbs. After oral administration of SND, 33 compounds and five metabolites in rat plasma were detected and identified by comparing and contrasting the compounds measured in SND with those in the plasma samples by HPLC/DAD/TOFMS. The results provided helpful chemical information for further pharmacology and active mechanism research on SND.
建立了一种高效液相色谱-二极管阵列检测-飞行时间质谱联用（HPLC/DAD/TOFMS）方法，以阐明四逆汤（SND）的化学成分以及口服SND后大鼠血浆中的化学成分。通过在TOFMS中动态调整碎裂电压，实现了离子的高效传输，从而获得最佳灵敏度，为每种分析物提供分子式，并为结构信息提供丰富的碎片离子。通过对每个分子离子及其后续碎片离子进行误差在5 ppm以内的精确质量测量，在SND中鉴定出53种化合物，包括二萜生物碱、黄酮类、三萜类和姜辣素相关化合物。从SND中鉴定出的主要化合物进一步在三味单味药中进行了归属。口服SND后，通过HPLC/DAD/TOFMS将SND中测得的化合物与血浆样品中的化合物进行比较和对比，检测并鉴定出大鼠血浆中的33种化合物和5种代谢产物。该结果为进一步开展SND的药理学和作用机制研究提供了有用的化学信息。
