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鸡骨草叶中N-反式对香豆酰酪氨酸的纯化工艺优化
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| 篇名： | 鸡骨草叶中N-反式对香豆酰酪氨酸的纯化工艺优化 |
| TITLE： | |
| 摘要： | 目的：建立鸡骨草叶中N-反式对香豆酰酪氨酸的含量测定方法，并优化其纯化工艺。方法：采用高效液相色谱法测定鸡骨草叶中N-反式对香豆酰酪氨酸的含量，色谱柱为Hypersil BDS C18，流动相为0.1％甲酸水溶液（A）-甲醇（B）（梯度洗脱），流速为1.0 mL/min，柱温为25 ℃，检测波长为300 nm，进样量为10 μL。以聚酰胺树脂为材料，以N-反式对香豆酰酪氨酸得率为指标，采用单因素试验优化N-反式对香豆酰酪氨酸纯化的样品溶液质量浓度、上样量、静置吸附时间等条件。结果：N-反式对香豆酰酪氨酸检测进样量线性范围为2.575～51.50 μg（r＝0.999 9）；定量限为0.000 618 μg，检测限为0.000 129 μg；精密度、稳定性、重复性试验的RSD均小于3％；加样回收率为97.04％～102.43％（RSD＝2.06％，n＝6）。最优纯化工艺为样品溶液质量浓度为0.04 g/mL（以鸡骨草叶药材计），上样量为50 mL，上样流速为1.0 mL/min，静置吸附时间为20 min，以水（含0.1％乙酸）、20％乙醇（含0.1％乙酸）、氨水（pH 10）为洗脱溶剂依次洗脱。此纯化工艺条件下，制得的N-反式对香豆酰酪氨酸的平均得率为98.94％，平均干膏含量为61.17 mg/g，平均干膏纯度为19.73％。结论：所建含量测定方法简便、准确、稳定性较好；优化所得工艺稳定、可行。 |
| ABSTRACT： | OBJECTIVE： To establish a method for content determination of N-（E）-p-coumaroyltyrosine in leaves of Abrus cantoniensis， and to optimize its purification technology. METHODS： HPLC method was adopted for the content determination of N-（E）-p-coumaroyltyrosine in A. cantoniensis. The determination was performed on Hypersil BDS C18 column with mobile phase consisted of 0.1％ formic acid water （A）-methanol （B） （gradient elution） at a flow rate of 1.0 mL/min. The column temperature was set at 25 ℃. The detection wavelength was set at 300 nm， and sample size was 10 μL. Using polyamide resin as material， the yield of N-（E）-p-coumaroyltyrosine as indicators， single factor test was used to optimize the purification technology of N-（E）-p-coumaroyltyrosine， such as concentration， sample size， stationary adsorption time. RESULTS： The linear range was 2.575-51.50 μg （r＝0.999 9） for N-（E）-p-coumaroyl-tyrosine. The limit of quantification was 0.000 618 μg， and the detection limit was 0.000 129 μg. RSDs of precision， stability and reproducibility tests were all lower than 3％. The recoveries were 97.04％-102.43％ （RSD＝2.06％， n＝6）. The optimal purification technology was as follows： the concentration of the sample solution was 0.04 g /mL （by the leaves of A. cantoniensis）； sample capacity 50 mL； the sample flow rate was 1.0 mL/min； the stationary adsorption time was 20 min； the eluting solvents were ammonia containing water （containing 0.1％ acetic acid）， 20％ ethanol （containing 0.1％ acetic acid） and ammonia（pH 10）. Average yield was 98.94％，average dry paste content was 61.17 mg/g， and average dry paste purity was 19.73％ by optimal purification technology. CONCLUSIONS： Established method is simple， accurate and stable. The optimized technology is stable and feasible. |
| 期刊： | 2019年第30卷第10期 |
| 作者： | 门丽娇，刘亚迪，邱雨，袁旭江 |
| AUTHORS： | MEN Lijiao，LIU Yadi，QIU Yu，YUAN Xujiang |
| 关键字： | 鸡骨草；叶；N-反式对香豆酰酪氨酸；高效液相色谱法；纯化工艺；柱层析法 |
| KEYWORDS： | Abrus cantoniensis； Leaves； N-（E）-p-coumaroyltyrosine； HPLC； Purification technology； Column chromatography |
| 阅读数： | 362 次 |
| 本月下载数： | 8 次 |
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