摘要: |
目的:应用高效液相色谱法测定中药材百部直立百部中2种有效生物碱成分(对叶百部烯酮、脱氢对叶百部碱)的含量。方法:采用高效液相色谱法,使用THERMO Hypersil ODS-C18色谱柱(250 mm×4.6 mm,2.5 μm),以乙腈0.2%甲酸氨缓冲溶液为流动相进行梯度洗脱(0~35 min,体积比为45∶55;35~55 min,体积比为45∶55~55∶45;55~70 min,体积比为55∶45),柱温为30℃,检测波长为235 nm,进样量为20 μl,流速为1.0 ml/min。结果:对叶百部烯酮的线性关系方程为:Y=0.9124×104X+3.9856×104(r=0.9998),脱氢对叶百部碱的线性关系方程为:Y=1.3062×104X+9.5647×104(r=0.9996),2种成分分别在0.0267~0.267、0.0235~0.1635 mg/ml范围内线性关系良好。对叶百部烯酮的平均加样回收率为99.71%,RSD为1.02%,脱氢对叶百部碱的平均加样回收率为99.91%,RSD为1.20%。结论:采用高效液相色谱法测定百部中药材中直立百部2种生物碱的含量,操作简便,检测方式简单,仪器精密度高,重现性好,可用于百部药材直立百部的质量控制。 |
关键词: 直立百部 生物碱 对叶百部烯酮 脱氢对叶百部碱 高效液相色谱法 实验研究 |
DOI: |
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Content determination of two alkaloids in the Chinese medicinal material Stemona sessilifolia by high-performance liquid chromatography |
ZHAO Xia,LIU Jinjin,ZHANG Guomin |
(Xiangcheng Institute for Food and Drug Control,Xiangcheng 461700,Henan,China;Changge Institute for Food and Drug Control,Changge 461500,Henan,China) |
Abstract: |
Objective:To determine the content of two effective alkaloids (tuberostemoenone and didehydrotuberostemonine) in the Chinese medicinal material Stemona sessilifolia by high-performance liquid chromatography (HPLC).Methods:HPLC was performed on a THERMO Hypersil ODS-C18column (250 mm×4.6 mm,2.5 μm) with a mobile phase of acetonitrile-0.2% methionine buffer solution for gradient elution (with a volume ratio of 45∶55 for 0~35 minutes,45∶55~55∶45 for 35~55 minutes,and 55∶45 for 55~70 minutes),at a column temperature of 30℃,a detection wavelength of 235 nm,a sample size of 20 μL,and a flow rate of 1.0 ml/min.Results:Tuberostemoenone showed a linear relationship with a regression equation of Y=0.9124×104X+3.9856×104 (r=0.9998),and didehydrotuberostemonine showed a linear relationship with a regression equation of Y=1.3062×104X+9.5647×104(r=0.9996);the two constituents showed a good linear relationship within the ranges of 0.0267~0.267 mg/mL and 0.0235~0.1635 mg/mL,respectively.Tuberostemoenone showed an average recovery rate of 99.71%,with a relative standard deviation of 1.02%,and didehydrotuberostemonine showed an average recovery rate of 99.91%,with a relative standard deviation of 1.20%.Conclusion:HPLC is simple and convenient and has good precision and repeatability in determining the content of the two alkaloids in the Chinese medicinal material Stemona sessilifolia,and therefore,it can be used for the quality control of Stemona sessilifolia. |
Key words: Stemona sessilifolia alkaloid tuberostemoenone didehydrotuberostemonine high-performance liquid chromatography experimental study |