School of Pharmacy, Shenyang Pharmaceutical University, Wenhua Road 103, Shenyang, 110016, China.
Rapid Commun Mass Spectrom. 2012 Oct 30;26(20):2443-53. doi: 10.1002/rcm.6360.
Liquid chromatography (LC) coupled to positive electrospray ionization (ESI) tandem mass spectrometry (MS/MS) employing a time-of-flight tandem mass spectrometer was established to identify multi-components of Zhi-zi-chi decoction, a traditional Chinese medicine formula, and the constituents in rat plasma after oral administration of Zhi-zi-chi decoction.
The LC separation was achieved on a C(18) column. The mobile phase consisted of acetonitrile/0.2% formic acid with gradient program. The quadrupole time-of-flight (Q-TOF) mass spectrometer was operated in the positive ion mode with an electrospray ionization source (ESI+). The capillary voltage of the ion source was set at 4500 V and the capillary exit was 90 V. The nebulizer pressure was maintained at 1.2 bar. Hexapole radio frequencies 1 and 2 were set to 200 Vpp and 250 Vpp, respectively.
A total 47 compounds in the Zhi-zi-chi decoction and 24 constituents in rat plasma after oral administration of Zhi-zi-chi decoction were identified. Of the 47 detected compounds in the Zhi-zi-chi decoction, 15 were identified by comparing the retention time and MS data with that of reference compounds and the rest were identified by MS analysis and retrieving the reference literature. Of the identified 24 compounds in rat plasma, 19 were the original form of the compounds absorbed from the 47 detected compounds, and the other five were the metabolites of the compounds existing in the Zhi-zi-chi decoction.
A fast and sensitive LC/Q-TOF MS method has been developed and successfully utilized to screen the active ingredients of a Chinese medical formula, Zhi-zi-chi decoction, for the first time. The results indicated that the 24 compounds identified in rat plasma were the potential active ingredients of Zhi-zi-chi decoction, which provided helpful chemical information for further pharmacology and active mechanism research on Zhi-zi-chi decoction and other traditional Chinese medicines.
采用正离子电喷雾串联质谱（ESI-MS/MS）-飞行时间串联质谱（TOF-MS/MS），建立一种用于鉴定中药栀子豉汤多成分的液相色谱（LC）方法，并检测栀子豉汤灌胃大鼠后血浆中的成分。
采用 C（18）柱进行 LC 分离，流动相为乙腈/0.2%甲酸，采用梯度洗脱程序。四极杆飞行时间（Q-TOF）质谱仪采用正离子模式（ESI+）进行检测，离子源的毛细管电压设定为 4500V，毛细管出口电压为 90V，雾化器压力为 1.2bar，离子阱射频 1 和射频 2 分别设定为 200Vpp 和 250Vpp。
在栀子豉汤中鉴定出 47 种化合物，在栀子豉汤灌胃大鼠血浆中鉴定出 24 种成分。在栀子豉汤中检测到的 47 种化合物中，有 15 种化合物通过比较保留时间和 MS 数据与对照品进行了鉴定，其余 32 种化合物通过 MS 分析和检索参考文献进行了鉴定。在大鼠血浆中鉴定出的 24 种成分中，有 19 种是从 47 种检测到的化合物中吸收的原型化合物，其余 5 种是栀子豉汤中存在的化合物的代谢物。
首次建立了快速灵敏的 LC/Q-TOF MS 方法，并成功应用于筛选中药栀子豉汤的活性成分。结果表明，在大鼠血浆中鉴定出的 24 种化合物可能是栀子豉汤的潜在活性成分，为进一步研究栀子豉汤及其他中药的药理学和作用机制提供了有价值的化学信息。
