摘要
目的优化D101大孔树脂分离连翘酯苷的条件和快速检测方法。方法连翘提取液经过D101大孔树脂吸附后,以不同浓度乙醇溶液洗脱,采用HPLC测定连翘酯苷的含量,并以测定值作参比,判定紫外扫描跟踪检测方法的可靠性。一次正交考察树脂用量、连翘提取液浓度、上样时间等因素对树脂吸附率的影响;二次正交考察乙醇浓度、洗脱液用量、洗脱速度对连翘酯苷纯度及树脂解吸率的影响,并绘制连翘酯苷的洗脱曲线。结果树脂用量对连翘酯苷吸附量影响极显著,最佳吸附条件为A2B3C2D2。最佳解吸条件根据考察指标不同有所差异,以纯度为指标时最佳条件为a2b1c1;以得率为指标时最佳条件为a3b1c3。洗脱液中含连翘酯苷时,紫外扫描图谱和连翘酯苷对照品的图谱基本一致。结论D101大孔树脂作为分离连翘酯苷较好的分离材料,对其进行优化的分离工艺可行;应用紫外扫描可快捷检测连翘酯苷的洗脱情况。
OBJECTIVE To research the optimized procedure of forsythiaside separation by D101 macroporous resin and detect it by ultraviolet spectrophotometry. METHODS The extraction solution of forsythia suspensa was absorbed by macroporous resin,and then the resin was eluted with different concentration alcohol. The contents of forsythiaside were determined by HPLC. HPLC assay was a reference method for the reliability of the ultraviolet spectrophotometry real-time tracking detection. The first orthogonal test investigated the effect of resin quantity,extract concentration and time on the adsorption of forsythiaside. The second orthogonal test investigated the effect of ethanol percentage,elution liquid quantity and flow rate on elution. The elution curve was obtained. RESULTS Resin quantity had significant influence on adsorption and the optimum adsorption condition were A2B3C2D2. The optimized elution condition was different according to purity or yield as index. The optimum condition for purity were a2b1c1. The optimum conditions for yield were a3b1c3. CONCLUSION Ultraviolet spectrophotometry can be used in real-time tracking detection of forsythiaside. D101 resin is suitable for the separation of forsythiaside. The optimized procedure is practical. The method of ultraviolet spectrophotometry detection with separation of forsythiaside by D101 macroporous resin is rapid.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2009年第22期1685-1688,共4页
Chinese Pharmaceutical Journal
基金
国家自然科学基金项目(30771625
30471306)
北京市自然科学基金(6053025)
北京市农委项目(20020103)
北京市教委项目(km20051002002)
北京市属高校人才强教深化计划(PHR2009-07135)
