玄参提取物化学成分及其大鼠血浆移行成分的LC―LTQ―Orbitrap分析[权威资料].docVIP

玄参提取物化学成分及其大鼠血浆移行成分的LC―LTQ―Orbitrap分析 　　[摘要]运用HPLC-LTQ-Orbitrap技术，分析玄参提取物体外化学成分及给药后大鼠血中移行成分。采用Venusil MP C色谱柱梯度洗脱进行分离，负离子模式下采集谱图。通过与文献及部分对照品比对，综合分析总离子流色谱图、提取离子流图以及质谱图等信息，对玄参提取物的化学成分及其血中移行成分进行定性研究。共推断出玄参提取物中37个化学成分，其中12个环烯醚萜苷类成分，20个苯丙素类成分，5个未知成分；确定哈巴苷、哈巴俄苷和安格洛苷C均以原型入血，并推测出其他2个原型成分及2个代谢产物。该研究能够为阐明玄参的药效物质基础提供一定依据，也对进一步研究玄参有重要意义。 　　[关键词]玄参；LC-LTQ-Orbitrap；化学成分；入血成分 　　[Abstract]Chemical constituents in extract of Scrophulariae Radix and their metabolites in rat plasma after oral administration were identified by HPLC-LTQ-Orbitrap. Samples were separated by a Venusil MP C column using a binary gradient elution. The information on the total ion chromatogram， the extraction chromatogram and the mass spectrogram in a negative mode were synthetically analyzed by comparing the retention time， MS and MS/MS spectra with literature data and some of reference standards to conduct a qualitative study on constituents of Radix Scrophulariae extract in vivo and in vitro. Totally 37 compounds from Scrophularia ningpoensis extract were detected including 12 iridoid glycosides， 20 phenylpropanoids and 5 unknown compounds. In vivo， harpagide， harpagoside and angoroside C were confirmed to enter into the blood in prototype forms. Besides， another 2 prototype compounds and 2 metabolites were detected in rat plasma after oral administration of S. ningpoensis extract. The results are beneficial for the determination of bioactive substances of S. ningpoensis and significant for further studies on S. ningpoensis. 　　[Key words]Scrophularia ningpoensis； LC-LTQ-Orbitrap； chemical component； constituents in plasma 　　玄参为玄参科植物玄参Scrophularia ningpoensis Hemsl.的干燥根，在我国药用历史悠久。初载于《神农本草经》，又称元参、黑参，味甘、苦、咸，归肺、胃、肾经，以根茎入药，具有凉血滋阴、泻火解毒的功效。 　　目前，有关玄参的研究主要集中在以下2个方面：其一是玄参及其复方制剂的含量测定和质量控制建立了快速测定大鼠血浆中哈巴俄苷、肉桂酸含量的LC-MS法，为二者药代动力学研究提供依据。但是，口服玄参后，玄参的血浆移行成分及其在体内的代谢转化目前仍然知之甚少。本文拟采用LC-LTQ-Orbitrap法，在负离子扫描模式下，对多个时间点的血浆混合样品进行检测和结构鉴定，并通过与对照品以及相关文献比对进一步确认所推断的结构。 　　1材料 　　Accela高效液相色谱仪与LTQ-Orbitr