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HPLC法测定圣愈汤冻干粉中4个指标成分的含量
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| 篇名： | HPLC法测定圣愈汤冻干粉中4个指标成分的含量 |
| TITLE： | Content Determination of 4 Indicator Components in Shengyu Decoction Lyophilized Powder by HPLC |
| 摘要： | 目的：建立测定圣愈汤冻干粉中阿魏酸、毛蕊花糖苷、藁本内酯、黄芪甲苷含量的方法。方法：采用高效液相色谱法测定3批冻干粉样品4种成分含量。测定阿魏酸、毛蕊花糖苷、藁本内酯的色谱柱为InertsilODS-SPC18，流动相为甲醇-0.1％磷酸水溶液，梯度洗脱，流速为1.0mL/min，检测波长为330nm，检测器为二极管阵列检测器，柱温为30℃，进样量为10μL；测定黄芪甲苷的色谱柱为KromasilC18，流动相为乙腈-水（32∶68，V/V），检测器为蒸发光散射检测器，漂移管温度为100℃，载气（空气）流量为2.5L/min，流速为1.0mL/min，柱温为30℃，进样量为10μL。结果：阿魏酸、毛蕊花糖苷、藁本内酯和黄芪甲苷进样量线性范围分别为0.05015～10.03μg（r＝0.9998）、0.06780～13.56μg（r＝0.9999）、0.05730～11.46μg（r＝0.9995）、1.128～11.28μg（r＝0.9993）；检测限分别为2.12×10－4、1.30×10－3、8.02×10－4、1.09×10－3μg，定量限分别为7.43×10－4、3.87×10－3、2.34×10－3、3.36×10－3μg；精密度、稳定性（12h）、重复性试验的RSD均小于2％（n＝6）；平均加样回收率分别为99.6％（RSD＝0.83％，n＝6）、100.9％（RSD＝1.07％，n＝6）、98.8％（RSD＝0.84％，n＝6）和101.3％（RSD＝0.99％，n＝6）。3批样品中阿魏酸、毛蕊花糖苷、藁本内酯和黄芪甲苷的含量分别为1.225～1.248、0.413～0.424、0.325～0.332、0.394～0.404mg/g（批间RSD＜1.5％）。结论：建立的含量测定方法稳定性、重复性好，能够快速、准确地测定圣愈汤冻干粉中阿魏酸、毛蕊花糖苷、藁本内酯和黄芪甲苷的含量。 |
| ABSTRACT： | OBJECTIVE：To establish the content determin ation method of ferulic acid ，verbascoside，ligustilide and astragaloside in Shengyu decoction lyophilized powder. METHODS ：HPLC method was adopted to determine 4 components in 3 batches of lyophilized powder. The determination of ferulic acid ，verbascoside and ligustilide was performed on Inertsil ODS-SP C 18 column with mobile phase consisted of methanol- 0.1％ phosphoric acid （gradient elution ）at the flow rate of 1.0 mL/min；detector was diode array detector ；detection wavelength was set at 330 nm；column temperature was 30 ℃，the sample size was 10 μL. The determination of astragaloside was performed on Kromasil C 18 column with mobile phase consisted of acetonitrile-water （32∶68，V/ V）；detector was evaporative light scattering detector ；the drift tube temperature wa s 100 ℃，the carrier gas （air）flow rate was 2.5 L/min at the flow rate of 1.0 mL/min；column temperature was 30 ℃，the sample size was 10 μL. RESULTS：The linear ranges of ferulic acid ，verbascoside，ligustilide and astragaloside were 0.050 15-10.03 μg（r＝0.999 8），0.067 80-13.56 μg（r＝ 0.999 9），0.057 30-11.46 μg（r＝0.999 5），1.128-11.28 μg（r＝0.999 3），respectively. The detection limits were 2.12×10－4，1.30× 10－3，8.02×10－4，1.09×10－3 μg，respectively. The limit of quantification were 7.43×10－4，3.87×10－3，2.34×10－3，3.36×10－3 μg， respectively. RSDs of precision ，stability（12 h）and reproducibility tests were all lower than 2％（n＝6）. Average recovery rates were 99.6％（RSD＝0.83％，n＝6），100.9％（RSD＝1.07％，n＝6），98.8％（RSD＝0.84％，n＝6）and 101.3％（RSD＝0.99％， n＝6），respectively. The contents of ferulic acid ，verbascoside，ligustilide and astragaloside in 3 batches of samples were 1.225-1.248， 0.413-0.424， 0.325-0.332， 0.394-0.404 mg/g， respectively （RSDs among batches were lower than 1.5％ ）. CONCLUSIONS：Established method is stable ，reproducible，rapid and accurate for the content determination of ferulic acid ， verbascoside， ligustilide and astragaloside in Shengyu |
| 期刊： | 2020年第31卷第05期 |
| 作者： | 董丹华，刘玉军，李亚男，胡祥昊，孙平，李婷，刘菊妍，高鹏 |
| AUTHORS： | DONG Danhua ，LIU Yujun，LI Yanan ，HU Xianghao ，SUN Ping，LI Ting，LIU Juyan，GAO Peng |
| 关键字： | 圣愈汤；冻干粉；高效液相色谱法；阿魏酸；毛蕊花糖苷；藁本内酯；黄芪甲苷；含量测定 |
| KEYWORDS： | Shengyu decoction ； Lyophilized powder ； |
| 阅读数： | 334 次 |
| 本月下载数： | 9 次 |
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