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目的应用高分离度快速液相-飞行时间质谱(RRLC-TOF/MS)联用技术鉴别防风入血成分及尿液中的原型成分及代谢产物,以探索防风可能的药效成分及体内代谢过程。方法采用Angilent Zorbax Extend-C18柱(250mm×4.6mm,5μmid),甲醇-水流动相体系梯度洗脱,在飞行时间质谱正离子模式下扫描,利用TOF/MS得到的准确相对分子质量,对照化学成分数据库,对血浆、尿液中的防风成分及代谢物进行鉴别。结果鉴别出血浆中6个防风原型成分:蔗糖、升麻苷、升麻素、紫花前胡苷元、5-O-甲基维斯阿米醇苷和3’-O-i-丁酰亥茅酚;尿液中8个原型成分:升麻苷、divaricatacid、升麻素、5-O-甲基维斯阿米醇苷、(3S)-2,2-二甲基-3,5-二羟基-8-羟甲基-3,4-二氢-2H,6H-苯并-[1,2-b:5,4-b’]双吡喃-6-酮、5-O-甲基维斯阿米醇、亥茅酚苷和汉黄芩素;及2个代谢产物:升麻素的葡萄糖醛酸苷和升麻素的同分异构体。结论该方法可靠、有效,可成功用于防风体内成分鉴别,并为进一步的药效实验提供参考和依据。
OBJECTIVE To identify the components and metabolites of anti-wind and blood components and urine samples by high-resolution rapid liquid phase-time of flight mass spectrometry (RRLC-TOF / MS) in order to explore the potential pharmacological components of windbreak and the metabolic processes in vivo . Methods Angilent Zorbax Extend-C18 column (250mm × 4.6mm, 5μmid) was used as the mobile phase of methanol-water mobile phase. The relative molecular mass of TOF / MS was obtained by scanning with time-of- Ingredient database for identification of anti-wind components and metabolites in plasma and urine. Results Six prototypes of the windproof prototype were identified: sucrose, aconitine, cimicifuga, purpurin, 5-O-methylvishisainin and 3’-Oi-butyrylhorseol; Eight prototype ingredients in solution: divaricatacid, cimiliren, 5-O-methylvishisainin, (3S) -2,2-dimethyl-3,5-dihydroxy-8 Hydroxymethyl-3,4-dihydro-2H, 6H-benzo- [1,2-b: 5,4-b ’ Galactin, menthol glycoside and wogonin; and two metabolites: glucuronide of cimorphine and isomers of cimorphine. Conclusion The method is reliable and effective and can be successfully used for identification of components in the windproof shelter and provide a reference and basis for further efficacy experiments.