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作 者:陈学国[1] 孔亮[1] 盛亮洪[2] 厉欣[1] 邹汉法[1]
机构地区:[1]中国科学院大连化学物理研究所国家色谱研究分析中心,辽宁大连116011 [2]中国药科大学生药学教研室,江苏南京210038
出 处:《色谱》2005年第1期46-51,共6页Chinese Journal of Chromatography
基 金:国家自然科学基金资助项目(90209056).
摘 要:建立了全二维液相色谱串联质谱分离分析模式,将质脂体色谱柱和ODS反相色谱柱作为二维分析色谱柱,二者通过一个连有两个0 5mL定量环的八通阀耦联。质脂体色谱柱上的馏分在反相色谱柱上分离后,直接进入紫外 检测器,然后经分流器分流后进入大气压电离质谱。将该体系用于银杏叶提取物的组成研究,共检测到至少41个组分,结合紫外 可见光谱和质谱信息,其中13个组分初步鉴定为银杏内酯B、银杏内酯C、白果内酯、槲皮素芸香糖苷、槲皮素、槲皮素 3 O β D 葡萄糖基(1 2) α L 鼠李糖苷、槲皮素 3 O β D 葡萄糖苷、异鼠李素、山柰酚 3 O β D 芸香糖基(1 2) α L 鼠李糖苷、异鼠李素 3 O β D 芸香糖苷、山柰酚 3 O β D 葡萄糖苷、山柰酚和山柰酚 3 O β D 芸香糖苷。A comprehensive two-dimensional liquid chromatographic separation system based on the combination of an immobilized liposome chromatographic (ILC) column and an ODS column was developed for the separation of components in Ginkgo biloba, a traditional Chinese medicine. Two columns were coupled by a two-position, eight-port valve equipped with two storage loops, and the system was controlled by a computer. The effluent was detected both by a diode array detector and by an atmospheric pressure chemical ionization (APCI) mass spectrometer. Under the optimization separation conditions with the separation system, more than 41 components in the methanol extract of Ginkgo biloba were resolved. According to their UV and mass spectra, 13 of them were preliminarily identified as ginkgolide B, ginkgolide C, bilobalide, rutin, quercetin, quercetin-3-O-β-D-glucosyl (1-2)-α-L-rhamnoside, quercetin-3-O-β-D-glucoside, isorhamnetin, kaempferol-3-O-β-D-glucosyl (1-2)-α-L-rhamnoside, isohamnetin-3-O-β-D-rutinoside, kaempferol-3-O-β-D-glucoside, kaempferol, kaempferol-3-O-β-D-rutinoside.
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