HPLC-ELSD法测定白英中碱苷A的含量Determination of content of glycoalkaloid A in Solanum lyratum Thunb.by HPLC-ELSD
齐伟,孙长山,马龄,张弘颖,杨红英,孙立新
QI Wei1,SUN Chang-shan1,MA Ling2,ZHANG Hong-ying3,YANG Hong-ying1,SUN Li-xin1(1.School of Pharmacy
摘要(Abstract):
目的研究白英化学成分,建立HPLC-ELSD法测定白英中碱苷A[3-O-β-D-glucopyranosyl-(1→2)-β-D-glucopyranosyl-(1→4)-β-D-galactopyranoside-(25ξ)-solanidan-3β,23β-diol]的含量的方法。方法采用硅胶、ODS柱色谱进行分离纯化。运用NMR数据及理化性质鉴定单体化合物的结构。色谱柱为Elite-ODS C18(200 mm×4.6 mm,5μm),流动相为乙腈-体积分数为0.02%三乙胺水溶液(体积比为56∶44),检测器漂移管温度为95℃,氮气流速2.3 L.min-1。结果从白英提取物中分离得到碱苷A。碱苷A在0.4~4.0μg线性关系良好(r=0.999 6),平均回收率为99.6%(RSD=2.0%)。结论HPLC-ELSD法可用于白英中碱苷A的测定。
Objective To study the chemical constituents of Solanum lyratum Thunb.and develop an HPLC-ELSD method for the determination of glycoalkaloid A[3-O-β-D-glucopyranosyl-(1→2)-β-D-glucopyranosyl-(1→4)-β-D-galactopyranoside-(25ξ)-solanidan-3β,23β-diol]in Solanum lyratum Thunb..Methods The constituents were separated and purified by silica gel and ODS chromatography,and the structure of glycoalkaloid A was identified by NMR and physicochemical property.The operation was carried out on a Elite-ODS C18(200 mm×4.6 mm,5 μm)column with the mobile phase consisting of a mixture of acetonitrile-0.02%(φ)triethylamine(V∶V=56∶44).The parameters of drift tube and gas flow rate of the detector were set at 95 ℃ and 2.3 L·min-1,respectively.Results Glycoalkaloids A was obtained from Solanum lyratum Thunb..The linear range of glycoalkaloids was 0.4-4.0 μg(r=0.999 6)and the average recovery was 99.6%(RSD=2.0%).Conclusions The method is found to be accurate,sensitive and reproducible.It can be used for the determination of the content of glycoalkaloid A in Solanum lyratum Thunb..
关键词(KeyWords):
白英;碱苷A;高效液相色谱法;蒸发光散射检测器
Solanum lyratum Thunb.;glycoalkaloid A;HPLC;ELSD
基金项目(Foundation): 辽宁省科技厅资助项目(2007226011);; 沈阳市科技局资助项目(1071164-9-00)
作者(Author):
齐伟,孙长山,马龄,张弘颖,杨红英,孙立新
QI Wei1,SUN Chang-shan1,MA Ling2,ZHANG Hong-ying3,YANG Hong-ying1,SUN Li-xin1(1.School of Pharmacy
DOI: 10.14066/j.cnki.cn21-1349/r.2010.04.005
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