CAJ | 학술논문

建立高速逆流色谱分离纯化杭白菊总黄酮结晶中芹菜素-7-O-芸香糖、木犀草素-7-O-葡萄糖、芹菜素-7-O-葡萄糖以及金合欢素-7-O-葡萄糖4种黄酮类化合物。高速逆流分离过程分为两步,分别采用乙酸乙酯-乙醇-水-乙酸(体积比4：1：5：0.2)和氯仿-甲醇-水(体积比4：3：2)两个体系。在第一步中,100 mg的总黄酮结晶分离得到了11.2 mg的芹菜素-7-O-芸香糖、15.3 mg的木犀草素-7-O-葡萄糖、28.2 mg的芹菜素-7-O-葡萄糖。然后收集到尾吹液,旋蒸至干得到35 mg的浸膏。在第二步中,当采用氯仿-甲醇-水(体积比4：3：2)体系时,从35 mg的浸膏中分离纯化得到14.5 mg的金合欢素-7-O-葡萄糖。4个化合物的纯度分别为99.4%、93.6%、99.1%和99.5%,电喷雾电离质谱和氢、碳核磁共振波谱鉴定化合物的结构。
건립고속역류색보분리순화항백국총황동결정중근채소-7-O-예향당、목서초소-7-O-포도당、근채소-7-O-포도당이급금합환소-7-O-포도당4충황동류화합물。고속역류분리과정분위량보,분별채용을산을지-을순-수-을산(체적비4：1：5：0.2)화록방-갑순-수(체적비4：3：2)량개체계。재제일보중,100 mg적총황동결정분리득도료11.2 mg적근채소-7-O-예향당、15.3 mg적목서초소-7-O-포도당、28.2 mg적근채소-7-O-포도당。연후수집도미취액,선증지간득도35 mg적침고。재제이보중,당채용록방-갑순-수(체적비4：3：2)체계시,종35 mg적침고중분리순화득도14.5 mg적금합환소-7-O-포도당。4개화합물적순도분별위99.4%、93.6%、99.1%화99.5%,전분무전리질보화경、탄핵자공진파보감정화합물적결구。
High-speed counter-current chromatography ( HSCCC) method for isolation and purification of flavonoids crystalloid, i. e. apigenin-7-O-rutinoside( I) , luteolin-7-O-glucoside( II) , apigenin-7-O-glucoside( III) and acacetin-7-O-glucoside( IV) from Chrysanthemum morifolium Ramat. was established successfully. The separation was performed in two steps with two different types of solvent systems: ethyl acetate-ethanol-water-acetic acid (4:1:5:0. 2, v/v) and chloroform-methanol-water (4:3:2, v/v). In the first separation step, 100 mg of the flavonoids crystalloid yielded 11. 2 mg of apigenin-7-O-rutinoside, 15. 3 mg of luteolin-7-O-glucoside, and 28. 2 mg of apigenin-7-O-glucoside. Then we collected tail blowing fluid and obtained 35 mg of extract by evaporation to dryness. In the second step, when we used [ chloroform-methanol-water (4:3:2, v/v)] solvent system to separate the 35 mg of extract, 14. 5 mg of acacetin-7-O-glucoside could be obtained. Their four compounds purities were 99. 4 %, 93. 6 %, 99. 1% and 99. 5%, respectively. Their structures were identified by ESI-MS, 1H NMR, and 13C NMR.