Isolation of mono-caffeoylquinic acids from tobacco waste using continuous resin-based pre-separation and preparative HPLC.
Isolation of mono-caffeoylquinic acids from tobacco waste using continuous resin-based pre-separation and preparative HPLC.
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DOI：
10.1002/jssc.201101055
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发表时间：
2012-06
影响因子：
3.1
通讯作者：
Jun Wang;Dingqiang Lu;Yao Liang;Hui Zhao;Min Luo;Xiuquan Ling;P. Ouyang
中科院分区：
文献类型：
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作者：
Jun Wang;Dingqiang Lu;Yao Liang;Hui Zhao;Min Luo;Xiuquan Ling;P. Ouyang
从烟草（Nicotiana tobaccum L.）使用连续树脂预分离和制备型高效液相色谱法（HPLC）对废物进行分析。烟草废料提取液经D101和XAD-4树脂柱连续预分离，得到总单咖啡酰奎尼酸，纯度为67.71%，回收率为90.06%。研究了制备型HPLC中流动相组成、pH、流速和上样量等因素对单咖啡酰奎尼酸3种异构体分离度和产率的影响。确定了最佳色谱条件为：以15%（v/v）甲醇-冰醋酸水溶液为流动相，流速为4.0 mL/min，流速为4.0 mL/min，检测波长为360 nm，移动的。从300 mg上样样品中，在单次运行中获得56.3 mg 3-O-咖啡酰奎宁酸、92.8 mg 5-O-咖啡酰奎宁酸和73.1 mg 4-O-咖啡酰奎宁酸，每种的HPLC纯度均超过98%。化合物的结构经ESI-MS、1H-NMR和13 C-NMR确证。
Three isomers of mono-caffeoylquinic acid, specifically, 3-O-caffeoylquinic acid, 4-O-caffeoylquinic acid and 5-O-caffeoylquinic acid, were successfully isolated from a crude extract of tobacco (Nicotiana tobaccum L.) wastes using continuous resin-based pre-separation and preparative high-performance liquid chromatography (HPLC). The extract of tobacco wastes was continuously pre-separated by resin-based columns packed with D101 and XAD-4, yielding total mono-caffeoylquinic acids with a purity of 67.71% and a recovery rate of 90.06%. Variables affecting resolution and productivity of three mono-caffeoylquinic acid isomers in preparative HPLC (i.e. mobile-phase composition, pH, flow rate and loading amount) were studied. The optimum chromatographic conditions were determined to be a mobile phase consisting of 15% (v/v) methanol and aqueous acetic acid with a pH of 4.5, a flow rate of 4.0 mL/min, a loading amount of 4 mL and a detection wavelength of 360 nm. From 300 mg of loading sample, 56.3 mg of 3-O-caffeoylquinic acid, 92.8 mg of 5-O-caffeoylquinic acid and 73.1 mg of 4-O-caffeoylquinic acid were obtained in a single run, each with a purity of over 98% by HPLC. The structures of the isolated compounds were elucidated by ESI-MS, (1) H-NMR and (13) C-NMR spectral data.