目的 建立超高效液相色谱-电化学检测法同时测定女贞子中羟基酪醇、红景天苷和酪醇3种成分的方法。方法 取女贞子药材粉末0.1 g经20 mL甲醇超声提取30 min,提取液再经0.22 μm滤膜过滤后上样进行色谱分离。以 ACQUITY UPLC HSS T3 柱(2.1 mm×100 mm,1.8 μm)为固定相,25 mmol·L-1乙酸铵溶液(pH 3.6)-甲醇=88∶12(V/V)为流动相。电化学检测器检测,库伦检测池第一通道电压为350 mV,第二通道为550 mV。结果 羟基酪醇、红景天苷和酪醇的质量浓度在0.1~10、1~50和0.1~8 mg·L-1内与其峰面积呈线性关系(r2>0.999 0),平均加标回收率分别为101.52%、102.15%和101.92%,相对标准偏差分别为3.64%、3.87%和4.54%。结论 使用超高效液相色谱-电化学检测法测定3种成分不仅灵敏度高,而且分析时间大大缩短,适合于女贞子中3种苯乙醇类化合物的测定。
Abstract
OBJECTIVE To establish an ultra-high performance liquid chromatography-electrochemical detection method for simultaneous determination of hydroxytyrosol, salidroside and tyrosol in Ligustri Lucidi Fructus. METHODS Ligustri Lucidi Fructus powder(0.1 g)was extracted ultrasonically for 30 min with 20 mL of methanol. The extract was filtered through microporous membrane of 0.22 μm and then separated by UPLC using an Acquity UPLC HSS T3 chromatographic column(2.1 mm×100 mm, 1.8 μm)as stationary phase and a mixture of 25 mmol·L-1 ammonium acetate solution(pH 3.6)-methanol=88∶12(V/V) as mobile phase.The potential of electrochemical detector was set at 350 mV in the first channel and 550 mV in the second channel. RESULTS The linear relationship between peak area and mass concentrations of hydroxytyrosol, salidroside and tyrosol was good in the ranges of 0.1-10, 1-50 and 0.1-8 mg·L-1, respectively(r2>0.999 0). The recoveries were 101.52%, 102.15% and 101.92% with RSDs of 3.64%, 3.87% and 4.54%, respectively. CONCLUSION This developed UPLC-ECD method for determination of three components in Ligustri Lucidi Fructus is sensitive, and the analysis time is greatly shortened.
关键词
超高效液相色谱法 /
电化学检测 /
女贞子 /
羟基酪醇 /
红景天苷 /
酪醇
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Key words
ultra-high performance liquid chromatography /
electrochemical detection /
Ligustri Lucidi Fructus /
hydroxytyrosol /
salidroside /
tyrosol
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中图分类号：
R284
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参考文献
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脚注
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基金
国家自然科学基金项目资助(81760652);贵州省科技厅基础研究项目资助(黔科合基础[2016]1172)
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