基于UPLC-ESI-Orbitrap-MS技術(shù)對金釵石斛生物堿的分析
發(fā)布時(shí)間:2018-06-10 17:12
本文選題:金釵石斛 + 倍半萜類生物堿; 參考:《中國實(shí)驗(yàn)方劑學(xué)雜志》2017年20期
【摘要】:目的:通過UPLC-ESI-Orbitrap-MS技術(shù)對金釵石斛生物堿的主要化學(xué)成分進(jìn)行分析。方法:采用Thermo Q Exactive四極桿-靜電場軌道阱高分辨質(zhì)譜-色譜聯(lián)用系統(tǒng)分析,以Hypersil Gold C18色譜柱(2.1 mm×150 mm,1.9μm)為固定相,流動(dòng)相0.1%甲酸水溶液(A)-乙腈(B)梯度洗脫(0~2 min,5%B,2~15 min,5%~95%B,15~17 min,95%B),流速0.3 m L·min~(-1),柱溫40℃,進(jìn)樣量2μL;質(zhì)譜條件采用電噴霧離子化(ESI)方式,在正離子模式下,以full scan/targeted-dd MS2掃描模式檢測,研究金釵石斛生物堿的主要化學(xué)成分。結(jié)果:通過與對照品比對、結(jié)合參考文獻(xiàn),分析多級質(zhì)譜數(shù)據(jù),根據(jù)化學(xué)成分的質(zhì)譜碎片,推測色譜峰對應(yīng)的化學(xué)結(jié)構(gòu),共歸屬8種倍半萜類金釵石斛生物堿,分別是石斛堿(dendrobine),mubironine B,石斛氨堿(dendramine),石斛醚堿(dendroxine),石斛酮堿(nobilonine),6-羥基金石斛堿(6-hydroxynobiline),N-異戊烯基石斛堿(N-isopentenyldendrobinium),N-異戊烯基-6-羥基石斛堿(N-isopentenyl-6-hydroxydendroxinium)。結(jié)論:建立了金釵石斛倍半萜類生物堿的主要化學(xué)成分的分析方法,為金釵石斛藥材的鑒別及質(zhì)量控制提供了科學(xué)依據(jù)。
[Abstract]:Aim: to analyze the main chemical constituents of Dendrobium nobile alkaloids by UPLC-ESI-Orbitrap-MS. Methods: Thermo Q active quadrupole and electrostatic field orbital trap high resolution mass spectrometry were used as stationary phase with Hypersil Gold C18 column 2.1 mm 脳 150 mm ~ (1.9 渭 m) as stationary phase, and Hypersil Gold C _ (18) column (2.1 mm 脳 150 mm ~ (1.9 渭 m) was used as stationary phase. The mobile phase (0.1% formic acid aqueous solution) was gradient eluted by AI-acetonitrile B) with a gradient elution of 0 ~ 2 min ~ 5 min ~ (5) and B ~ (95) B ~ (15) ~ (17) min ~ (95) B ~ (-1), the flow rate was 0.3 mL / L, the column temperature was 40 鈩,
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