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HPLC-DAD-ELSD法测定黄芪经九州虫草双向固体发酵前后8种成分的含量
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| 篇名： | HPLC-DAD-ELSD法测定黄芪经九州虫草双向固体发酵前后8种成分的含量 |
| TITLE： | Content Determination of 8 Components in Astragalus membranaceus before and after Bidirectional Solid Fer- mentation with Cordyceps kyushuensis by HPLC-DAD-ELSD |
| 摘要： | 目的：建立同时测定黄芪经九州虫草双向固体发酵前后毛蕊异黄酮苷、芒柄花苷、毛蕊异黄酮、芒柄花素、黄芪皂苷Ⅳ、异黄芪皂苷Ⅱ、环黄芪醇、异黄芪皂苷Ⅰ等8种成分含量的方法，并探讨发酵处理对黄芪中上述8种成分含量的影响。方法：采用高效液相色谱-二极管阵列检测器-蒸发光检测器联用技术（HPLC-DAD-ELSD）进行含量测定。色谱柱为Agilent5TC-C18；流动相为0.1％甲酸水溶液（A）-乙腈（B），梯度洗脱；流速为1mL/min；柱温为30℃；DAD检测波长为260nm；ELSD蒸发管温度为100℃；雾化器温度为80℃；载气流速为1.6L/min；进样量为15μL。结果：8种成分在各自质量浓度范围内线性关系良好（R2均大于0.9990）；精密度、稳定性、重复性试验的RSD均小于3％（n＝3或n＝6）；平均加样回收率为97.88％～101.32％，RSD为1.22％～2.39％（n＝6）。以未发酵黄芪中相应成分含量为100％计算，经九州虫草双向固体发酵后，黄芪中毛蕊异黄酮苷、芒柄花苷、毛蕊异黄酮、芒柄花素、黄芪皂苷Ⅳ、异黄芪皂苷Ⅱ、环黄芪醇、异黄芪皂苷Ⅰ的含量变化率分别为－98.51％、－96.41％、－94.74％、－96.40％、289.20％、20.25％、－75.05％、562.46％。结论：黄芪经过九州虫草发酵后，有利于增加其主要活性成分黄芪皂苷Ⅳ、异黄芪皂苷Ⅰ、异黄芪皂苷Ⅱ的含量。 |
| ABSTRACT： | OBJECTIVE：To establish a method for simultaneous determination of calycosin glucoside ，ononin，calycosin， formononetin，astragaloside Ⅳ，isoastragaloside Ⅱ，cycloastragenol and isoastragaloside Ⅰ in Astragalus membranaceus before and after bidirectional solid fermentation with Cordyceps kyushuensis ，and to investigate the effects of fermentation on the contents of above 8 components in A. membranaceus . METHODS ：HPLC-DAD-ELSD was adopted. The determination was performed on Agilent 5 TC-C18 column with mobile phase consisted of 0.1％ formic acid aqueous solution-acetonitrile （gradient elution ）at the flow rate of 1 mL/min. The column temperature was set at 30 ℃. DAD detection wavelength was set at 260 nm，ELSD evaporation tube temperature was 100 ℃，atomizer temperature was 80 ℃，carrier gas flow rate was 1.6 L/min；injection volume was 15 μL. RESULTS：The eight components had a good linear relationship within their respective ranges of concentration （all R2＞0.999 0）； RSDs of precision ，stability and repeatability tests were all less than 3％（n＝3 or n＝6）；the recoveries was 97.88％-101.32％， and RSDs were 1.22％-2.39％（n＝6）. Setting the content of components in unfermented A. membranaceus as 100％，after bidirectional solid fermentation with C. kyushuensis ，the change rates of 8 components were －98.51％，－96.41％，－94.74％， －96.40％，289.20％，20.25％，－75.05％，562.46％，respectively. CONCLUSIONS ：After fermentation with C. kyushuensis ，the contents of active components as astragaloside Ⅳ，isoastragaloside Ⅰ and isoastragaloside Ⅱ can be increased significantly in A. membranaceus . |
| 期刊： | 2020年第31卷第23期 |
| 作者： | 杜以晴，于钦辉，文冉，菅彤彤，容蓉，吕青涛，张国英 |
| AUTHORS： | DU Yiqing ，YU Qinhui ，WEN Ran，JIAN Tongtong ，RONG Rong，LYU Qingtao ，ZHANG Guoying |
| 关键字： | 黄芪；九州虫草；双向固体发酵；高效液相色谱-二极管阵列检测器-蒸发光检测器联用技术；含量测定 |
| KEYWORDS： | Astragalus membranaceus ；Cordyceps kyushuensis ；Bidirectional solid fermentation ；HPLC-DAD-ELSD；Content |
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