摘要
采用高效液相色谱-二极管阵列检测-电喷雾质谱(HPLC-PAD-ESI-MS)法对开环异落叶松树脂酚二葡萄糖苷(SDG)进行定性和定量检测,研究方法的精密度、稳定性、定量检测限及加样回收率,并考察样品制备方法对定量检测结果的影响.采用Sephadex LH-20柱色谱分离制备SDG对照品,并用1H-NMR与13C-NMR对其进行表征.HPLC-PAD-ESI-MS检测所得紫外及电喷雾质谱信息与SDG结构相符.以自制的SDG(纯度96.6%)为对照,采用HPLC绘制定量标准曲线,方法精密度较高(RSD为1.36%),稳定性好(1周后RSD为1.21%),定量检测限较低(LOQ为3.4 mg·L-1),加样回收率达(99.7±3.2)%.此外,制样时采用碱法水解与混合溶剂提取,不仅节省时间,还更充分地提取了SDG.说明用HPLC-PAD-ESI-MS法检测亚麻籽中的SDG方便省时,准确可靠.
High performance liquid chromatography-photodiode array detection elctrospray ionizationmass spectrometry （HPLC PAD-ESI-MS） method was used to determine secoisolariciresinol diglucoside （SDG） qualitatively and quantitatively. Precision, stability, limits of quantification, SDG recovery and sample preparation method were studied. SDG was isolated on a Sephadex 1,H 20 column chromatography and characterized by I H-NMR and 13 C-NMR. Calibration curve was built with the purified SDG （with purity of 96.60/00） as a standard. The UV spectrum and ESI-MS spectra were in accordance with SDG structure. The HP1,C-PAD-ESI MS method had high precision （RSD 1.36%）, good stability （RSD 1.21% after a week）, low limit of quantification （3.4 mg·L^-1） and satisfying recovery （99.7 ± 3.2） %. In addition, by combination of solvent extraction with alkaline hydrolysis,sample preparation time was saved and SDG yield was improved. This HPLC-PAD-ESI-MS method is convenient, time-saving, accurate and reliable.
出处
《浙江大学学报（农业与生命科学版）》
CAS
CSCD
北大核心
2008年第5期564-570,共7页
Journal of Zhejiang University:Agriculture and Life Sciences
基金
江南大学2007年博士启动基金资助项目
