| 摘要: |
| 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(250 mm×4.6 mm,5 μm id),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。 |
| 关键词: 快速液相-飞行时间质谱法 防风 血浆 尿 代谢产物 |
| DOI：10.3724/SP.J.1008.2010.0760 |
| 投稿时间：2010-03-09修订日期：2010-06-08 |
| 基金项目: |
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| RRLC-TOF/MS in identification of constituents and metabolites of Radix Saposhnikoviae in rat plasma and urine |
| LI Yue-yue1, WANG Hui1, CHEN Jun1, ZHAO Liang1, ZHANG Hai1, CHAI Yi-feng2, ZHANG Guo-qing1*,ZHANG Guo-qing |
| (1.Department of Pharmacy, Eastern Hepatobiliary Surgery Hospital, Second Military Medical University, Shanghai 200438, China; 2.Department of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, Shanghai 200433, China) |
| Abstract: |
| ObjectiveTo analyze the constituents and metabolites of Radix Saposhnikoviae(RS) in rat plasma and urine by rapid-resolution liquid chromatography-time of flight mass spectrometry (RRLC-TOF/MS), so as to explore the active ingredients and metabolites of RS in vivo.MethodsThe separation was performed on a Angilent Zorbax Extend-C18 (5 μm, 250 mm×4.6 mm id) column, with a methanol-water mobile phase system used for gradient elution.Time-of-flight mass spectrometer (TOF/MS) was applied for qualitative analysis under positive ion mode.Based on the accurate molecular weight of TOF/MS detection and the compound list of RS established previously, the constituents and metabolites of RS in different matrix in vivo were identified.ResultsSix constituents of RS were identified in the plasma:sucrose, prim-O-glucosylcimifugin, cimifugin, nodakenetin, 5-O-methylvisamminol, and 3’-O-i-butyrylhammaudol.Eight constituents were identified in the urine:prim-O-glucosylcimifugin, divaricatacid, cimifugin, 4’-O-glucosyl-5-O-methylvisamminol, (3S)-2,2-dimethyl-3,5-dihydroxy-8-hydroxymethyl-3,4-dihydro-2H,6H-benzo-\[1,2-b:5,4-b’\]dipyran-6-one, 5-O-methylvisamminol, sec-O-β-D-glucosylhammaudol, and wogonin.Two metabolites were identified in the urine:glucuronide of cimifujin and an isomer of it.ConclusionThe present method is reliable and effective for identifying compounds of RS in vivo, and it can provide a reference and evidence for the further pharmacodynamics experiments. |
| Key words: rapid-resolution liquid chromatography-time of flight mass spectrometry Radix Saposhnikoviae plasma urine metabolites |
