[关键词]
[摘要]
目的 采用UPLC-Q-TOF-MS对大鼠ig消痔丸吸收入血成分进行鉴定。方法 采用Waters Acquity UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7 μm),流动相为0.1%甲酸水–甲醇,梯度洗脱,体积流量0.3 mL/min,柱温25 ℃,进样量5 μL。采用电喷雾离子源,正负离子模式,质量数扫描范围m/z 100~1 200;离子源温度100 ℃,脱溶剂气流温度250 ℃;毛细管电压正离子模式3.0 kV,负离子模式2.5 kV,样品锥孔电压40 V,锥孔气流速50 L/h,脱气流速600 L/h;内参校准液亮氨酸脑啡肽用于相对分子质量实时校正。结果 共识别出16种原型入血成分,鉴定出15种消痔丸的代谢产物。推断了木兰花碱、芹菜素、高良姜素、白术内酯II、毛蕊异黄酮葡萄糖苷、粉防己碱、小檗碱、染料木素在大鼠体内可能的代谢途径。结论 UPLC-Q-TOF-MS分析技术可快速鉴定大鼠ig消痔丸后血浆中化学成分,为挖掘消痔丸的药效物质提供依据。
[Key word]
[Abstract]
Objective To identify the absorbed blood constituents in rat after ig administrated with Xiaozhi Pills using UPLC-Q-TOF-MS method. Methods Waters Acquisition UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm) was used. The mobile phase consisted of 0.1% formic acid water and methanol with gradient elution at a flow rate of 0.3 mL/min. The column temperature was maintained at 25 ℃, and the injection volume was 5 μL. Mass spectrometric detection was carried out using an electrospray ion (ESI) source in positive and negative ion modes, and the mass scanning range was m/z 100 — 1 200. Ion source temperature was 100 ℃, and desolvation gas flow temperature was 250 ℃. Capillary voltage in positive ion mode was set at 3.0 kV and 2.5 kV in negative mode. The sample cone voltage was 40 V, the cone gas flow rate was 50 L/h, and degassing flow rate was 600 L/h. Internal reference calibration solution leucine enkephalin was used for real-time correction of relative molecular weight. Results A total of 16 prototype blood components and 15 metabolites of Xiaozhi Pills were identified. The proposed metabolic pathways of magnolol, apigenin, galangin, atractylenolide II, calycosin 7-O-β-D-glucopyranoside, tetrandrine, berberine, and genistein in rats were inferred. Conclusion UPLC-Q-TOF-MS method can quickly identify the chemical components in the plasma of rats after ig administrated with Xiaozhi Pills, providing a basis for exploring the pharmacological substances of Xiaozhi Pills.
[中图分类号]
R284.1
[基金项目]
甘肃省重点人才项目(2025RCXM029)