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基质固相分散结合高效液相色谱法测定狼毒大戟中jolkinolide A和jolkinolide B的方法研究

Development of matrix solid-phase dispersion coupled with high-performance liquid chromatography for determination of jolkinolide A and jolkinolide B in Euphorbia fischeriana Steud.

作者信息

Cai Defu, Zhai Weiyu, Zhang Qi, Liu Jianhua, Sun Yu, Liu Lei, Liu Jicheng

机构信息

a Institute of Medicine and Drug Research , Qiqihar Medical University , Qiqihar , China.

b The First Affiliated Hospital , Qiqihar Medical University , Qiqihar , China.

出版信息

Nat Prod Res. 2017 Aug;31(15):1805-1811. doi: 10.1080/14786419.2017.1297993. Epub 2017 Mar 24.

Abstract

A novel and simple method was established for the extraction and determination of jolkinolide A and B in Euphorbia fischeriana Steud. using matrix solid-phase dispersion (MSPD) extraction and high-performance liquid chromatography (HPLC). The optimised conditions for the MSPD extraction were determined to be that silica gel was served as dispersant, the mass ratio of sample to silica gel was selected to be 1:4, and 5 mL of acetonitrile was used as elution solvent. The method exhibited a good performance in terms of linearity (r ≥ 0.9997) and the limits of detection in the range of 0.052-0.065 μg mL. The recoveries were in the range of 90.2-98.9% with relative standard deviations (RSDs) ranging from 1.3 to 3.5%. The extraction efficiencies obtained by the MSPD were higher than other extraction method with less cost of sample and solvent. At last, the optimised method was applied for analysing real samples.

摘要

建立了一种新颖且简单的方法,用于采用基质固相分散(MSPD)萃取和高效液相色谱(HPLC)法提取和测定狼毒大戟中的jolkinolide A和B。MSPD萃取的优化条件确定为:以硅胶作为分散剂,样品与硅胶的质量比选择为1:4,并用5 mL乙腈作为洗脱溶剂。该方法在线性方面表现良好(r≥0.9997),检测限在0.052 - 0.065 μg/mL范围内。回收率在90.2% - 98.9%之间,相对标准偏差(RSD)为1.3% - 3.5%。MSPD获得的萃取效率高于其他萃取方法,且样品和溶剂成本更低。最后,将优化后的方法应用于实际样品分析。

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