山东科学
山東科學
산동과학
SHANDONG SCIENCE
2011年
6期
36-38,61
,共4页
董红敬%张永清%庄会永%李佳%耿岩玲%王晓
董紅敬%張永清%莊會永%李佳%耿巖玲%王曉
동홍경%장영청%장회영%리가%경암령%왕효
广西地不容%青风藤碱%pH区带精制逆流色谱法
廣西地不容%青風籐堿%pH區帶精製逆流色譜法
엄서지불용%청풍등감%pH구대정제역류색보법
Stephania kwangsiensis%Sinoacutine%pH-zone-refining counter-current chromatography
采用pH区带精制逆流色谱法从广西地不容中制备青风藤碱,溶剂系统为石油醚-乙酸乙酯-甲醇-水(3:7:1:9,V/V),上相加10mmol/L三乙胺为固定相,下相加10mmol/L盐酸为流动相。一次进样1.0g,可得纯度为99.5%的青风藤碱600mg,所得产物经ESI-MS,1H NMR和13C NMR进行结构鉴定。本方法效率高,制品纯度高,适合青风藤碱的大量制备。
採用pH區帶精製逆流色譜法從廣西地不容中製備青風籐堿,溶劑繫統為石油醚-乙痠乙酯-甲醇-水(3:7:1:9,V/V),上相加10mmol/L三乙胺為固定相,下相加10mmol/L鹽痠為流動相。一次進樣1.0g,可得純度為99.5%的青風籐堿600mg,所得產物經ESI-MS,1H NMR和13C NMR進行結構鑒定。本方法效率高,製品純度高,適閤青風籐堿的大量製備。
채용pH구대정제역류색보법종엄서지불용중제비청풍등감,용제계통위석유미-을산을지-갑순-수(3:7:1:9,V/V),상상가10mmol/L삼을알위고정상,하상가10mmol/L염산위류동상。일차진양1.0g,가득순도위99.5%적청풍등감600mg,소득산물경ESI-MS,1H NMR화13C NMR진행결구감정。본방법효솔고,제품순도고,괄합청풍등감적대량제비。
We employed pH-zone refining counter-current chromatography to prepare high-purity sinoacutine from Stephania kwangsiensis. Its solvent system was composed of petroleum ether-ethyl acetate-methanol-water (3 : 7: 1 : 9, V/V), in which triethylamine ( 10 mmol/L) was added to the upper organic stationary phase as a retainer and hydrochloric acid (10 mmol/L) was added to the aqueous mobile phase as an eluter. The structure of sinoautine was identified by ESI-MS,1H NMR and 13C NMR. The purity of sinoacutine determined by RP-HPLC was 99.5%. This approach has such advantages as high-efficiency and high-purity, suitable for the preparation of large amount of sinoacutine.