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HPLC-MSn法分析当归乙酸乙酯提取物在大鼠体内的代谢产物 被引量:7

Analysis of the Metabolites of Ethyl Acetate Extract from Angelica sinensis in Rats by HPLC-MSn
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摘要 目的:探讨当归乙酸乙酯提取物的抗凝血活性药效物质及其显效形式。方法:采用高效液相色谱-二极管阵列-电喷雾飞行时间质谱联用(HPLC-DAD-ESI-IT-TOF-MSn)技术对当归乙酸乙酯提取物的化学成分进行鉴别,并对其在大鼠体内的代谢产物进行分析。色谱柱为Agilent Zorbax SB-C18(250 mm×4.6 mm,5μm),柱温为28℃,流动相为0.1%甲酸水-甲醇(梯度洗脱),流速为1.0 ml/min,检测波长为280 nm。结果:通过对当归乙酸乙酯提取物的成分进行分析,共指认出22个化合物,其中当归相关研究中首次报道的化合物为4,7-二羟基-3-丁基苯酞;从大鼠含药尿液中共指认出18个化合物,包括原形成分4个,以及当归相关研究中首次报道的代谢产物14个,其中新化合物2个,分别为N,N-4,5-alkene-ligustilide-6/7-O-sulphate和6,7-dihydrosenkyunolide F-9-sulphate-6/7-thiol。结论:该方法能准确、快速地从复杂的生物样品中筛选和鉴定相关代谢产物,可为阐明当归抗凝血活性的药效物质及显效形式(原形、代谢产物或两者兼有)提供化学依据。 OBJECTIVE:To analyze the anticoagulant activity substance and effective form of ethyl acetate extract from Angeli- cae sinensis in rats. METHODS: The chemical constituents of ethyl acetate extract from A. sinensis were identified by HPLC-DAD-ESI-IT-TOF-MSn, and the in vivo metabolites of ethyl acetate extract were analyzed. The determination was performed on Agilent Zorbax SB-C18(250 mm×4.6 mm, 5 μm) column, using 0.1% formic acid-methanol as mobile phase (gradient elution) at a flow rate of 1.0 ml/min. The column temperature was 28 ℃, and UV detection was set at 280 nm. RESULTS: By analyzing ethyl acetate extract from A. sinensis, 22 compounds were detected and identified; among them, 4,7-dihroxyl-3-butylphthalide was reported for the first time. And 18 compounds were detected and identified in rat urine, containing 4 prototype and 14 metabolites reported for the first time, among which, N, N-4,5-alkene- ligustilide-6/7-O-sulphate and 6, 7-dihydrosenkytmolide F-9-sulphate-6/ 7-thiol were new compounds. CONCLUSIONS: The method can screen and identify related metabolites from complex biological specimens accurately and rapidly, and provide chemical evidence for interpreting effective forms and pharmacodynamic substances of A. sinensis anticoagulant activity.
出处 《中国药房》 CAS CSCD 2014年第47期4425-4430,共6页 China Pharmacy
关键词 当归 乙酸乙酯提取物 高效液相色谱-二极管阵列-电喷雾飞行时间质谱 代谢产物 药效物质 Angelicae sinensis Ethyl acetate extract HPLC-ESI-IT-TOF-MSn Metabolites Pharmacodynamic substances
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