摘要
样品经乙醇萃取后,提取液采用电动进样引入毛细管中进行毛细管电泳(CE)分离,进样电压为10kV,进样时间为10s。CE运行缓冲溶液为pH 5.13的10mmol·L^(-1)磷酸盐缓冲溶液,分离电压为15kV。CE分离得到的石斛碱与电化学发光(ECL)检测池中的5 mmol·L^(-1)Ru(bpy)_3^(2+)溶液(溶剂为pH 8.10的70 mmol·L^(-1)磷酸盐缓冲溶液)反应,使得Ru(bpy)_3^(2+)的ECL强度增大,检测电位为1.17V(vs.Ag/AgCl)。石斛碱的质量浓度在1.0~100mg·L^(-1)内与ECL信号的峰面积呈线性关系,检出限(3S/N)为0.045mg·L^(-1)。方法用于测定金钗石斛中石斛碱的含量,加标回收率在92.0%~105%之间,测定值的相对标准偏差(n=5)在2.5%~5.1%之间。
After the sample was extracted with ethanol,the extract was injected to the capillary for capillary electrophoresis（CE）separation by electric sampling for 10 swith the injection voltage of 10 kV.The running buffer solution for CE was 10mmol·L^-1 PBS（pH 5.13）and the separation voltage was 15 kV.The dendrobine after CE separation reacted with 5 mmol· L^-1 Ru（bpy）3^2＋ solution （in 70 mmol· L^-1 PBS with pH 8.10） in electrochemiluminescence（ECL）detection cell,resulting the ECL intensity of Ru（bpy）3^2＋ increaced at the detection potential of 1.17V（vs.Ag/AgCl）.Linear relationship was found between the peak area of ECL signal with the mass concentration of dendrobine in the range of 1.0-100 mg·L^-1,with detection limit （3S/N）of 0.045mg·L^-1.The proposed method was applied to the determination of dendrobine in Dendrobium nobile Lindl,giving recovery rates obtained by standard addition method in the range of 92.0%-105% and RSDs （n=5） were in the range of 2.5%-5.1%.
出处
《理化检验（化学分册）》
CSCD
北大核心
2017年第9期997-1001,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
广西壮族自治区自然科学基金(0640038)
北部湾红树植物白骨壤叶生物碱的分离纯化及抗菌活性项目(2D2014041)
关键词
毛细管电泳
电化学发光法
石斛碱
金钗石斛
capillary electrophoresis
electrochemiluminescence
dendrobine
Dendrobium nobile Lindl
