胡淑曼,付志飞,魏宝红,等.HPLC法测定海藻药材质量标志物岩藻糖的含量[J].中国海洋药物,2021,40(1):11-15. |
HPLC法测定海藻药材质量标志物岩藻糖的含量 |
Determination of Characteristic Ingredient-fucose in Marine TCM Sargassum by HPLC |
投稿时间:2020-04-24 修订日期:2020-05-13 |
DOI: |
中文关键词: 海藻药材 岩藻糖 柱前衍生高效液相色谱法 含量测定 |
English Keywords:Sargassum fucose precolumn derivatived-HPLC quantitative analysis |
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中文摘要: |
目的 建立中药海藻药材岩藻糖含量的HPLC测定方法。方法 水提得海藻粗多糖,继而经2 mol/L三氟乙酸降解、1-苯基-3-甲基-5-吡唑啉酮衍生后,采用HPLC测定岩藻糖含量,并进行方法学考察。结果 岩藻糖在6.44 ~ 824.52 μg/mL 浓度范围内具有良好的线性关系,y = 15.074 x - 52.068,r = 0.9998;最低检测限0.80 μg/mL,最低定量限1.61 μg/mL;供试品溶液在40 h内稳定性良好,RSD 0.04%;精密度、重复性良好,RSD分别为0.51%、1.15%;平均加样回收率为99.28 %,RSD 2.15 %(n = 9)。结论 建立的方法简便准确、精密度高、重复性好,可用于海藻药材的质量控制。 |
English Summary: |
Objective To establish a method for the determination of fucose in marine TCM Sagassum by performance liquid chromatography (HPCL). Methods The polysaccharides were prepared by water extraction. After degradated by 2 mol/L trifluoroacetic acid and derivatived by 1-phenyl-3-methyl-5-pyrazolone, an HPLC method has been developed for determination of fucose. Results The linear ranges were 6.44~824.52 μg/mL (y=15.074x-52.068,r=0.9998) with the limits of detection 0.80 μg/mL and quantification 1.61 μg/mL. Good precision (RSD 0.51 %, n=6)、repeatability (RSD 1.15 %, n=6) and stability( 40h in room temperature) were found. The average recovery rate was 99.28 % (RSD 2.15 %, n=9). Conclusion The established method was simple, accurate and reproducible, which could provide the reference for the quality control of marine TCM Sargassum. |
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