MSPD-UPLC法同时测定狼毒大戟中4种成分  

Simultaneous determination of four compounds in Euphorbia fischeriana by MSPD-UPLC

作　　者：刘雷[1] 马玉坤[1] 孙宇[1] 刘琦 张金玲[1] 郭丽娜[1] 刘吉成[1] LIU Lei;MA Yu-kun;SUN Yu;LIU Qi;ZHANG Jin-ling;GUO Li-na;LIU Ji-cheng(Qiqihar Medical University,Qiqihar 161006,China)

机构地区：[1]齐齐哈尔医学院,黑龙江齐齐哈尔161006

出　　处：《中成药》2020年第6期1520-1525,共6页Chinese Traditional Patent Medicine

基　　金：国家自然科学基金资助项目(81573660);黑龙江省教育厅科学技术研究项目(2017-KYYWF-0702)。

摘　　要：目的建立基质固相分散-超高效液相色谱法(MSPD-UPLC)测定狼毒大戟Euphorbia fischeriana Steud.中岩大戟内酯A、17-羟基-岩大戟内酯A、岩大戟内酯B、17-羟基-岩大戟内酯B的含有量。方法样品前处理采用MSPD法,以硅胶为分散剂,乙腈为洗脱溶剂;样品分析采用Waters BEH C18色谱柱(2.1 mm×50 mm,1.7μm);流动相乙腈-水,梯度洗脱;体积流量0.4 mL/min;检测波长250 nm;柱温35℃。结果各目标分析物在各自范围内具有良好的线性关系(r≥0.999 5),检出限与定量限分别介于0.072~0.78μg/mL和0.24~2.61μg/mL之间,平均加样回收率93.0%~94.4%。结论该法操作简单、溶剂用量少、分析时间短,可用于狼毒大戟中活性成分的提取与检测。AIM To establish an MSPD-UPLC method for the simultaneous content determination of jolkinolide A,17-hydroxyjolkinolide A,jolkinolide B,17-hydroxyjolkinolide B in Euphorbia fischeriana Steud. METHODS The samples were prepared by an optimized MSPD procedure using silica as the dispersant and acetonitrile as the elution solvent. The analysis of samples was performed on a 35 ℃ thermostatic Waters BEH C18column(2.1 mm×50 mm, 1.7 μm), with the mobile phase comprising of acetonitrile-water flowing at 0.4 mL/min in a gradient elution manner,and the detection wavelength was set at 250 nm. RESULTS The target analyte showed good linear relationships within their own ranges(r>0.999 5), whose average recoveries were 93.0%-94.4%. The limits of detection(LODs) and quantification(LOQs) were in the range of 0.072-0.78 μg/mL and 0.24-2.61 μg/mL. CONCLUSION This method is simple and timesaving with reduced requirements on the amount of sample and solvent,and can be used for the extraction and determination of E. fischeriana.

关 键 词：狼毒大戟 基质固相分散萃取 超高效液相色谱 岩大戟内酯A 17-羟基-岩大戟内酯A 岩大戟内酯B 17-羟基-岩大戟内酯B 

分 类 号：R284􀆰[医药卫生—中药学]