摘要
目的建立鲜百合质量控制方法。方法采用TLC法对鲜百合进行定性鉴别,HPLC法测定王百合苷B含量;参照2015年版《中国药典》方法,测定水分、总灰分和浸出物含量。结果TLC定性鉴别采用硅胶G板,以石油醚-二氯甲烷-乙酸乙酯-甲醇(7∶10∶7∶2)为展开系统,10%硫酸乙醇显色,365 nm下检视:鲜百合样品与对照药材在相同位置呈现相同颜色斑点,斑点清晰,重复性好;HPLC含量测定采用Agilent C18色谱柱(4.6 mm×250 mm,5μm),在流动相乙腈-0.1%磷酸(17∶83)、检测波长312 nm、柱温25℃、流速1.0 mL/min、进样量20μL条件下,王百合苷B在10.27~164.32 mg/L范围内线性关系良好(R^2=0.9997),平均加样回收率为100.08%(RSD为2.31%)。20批样品中,王百合苷B含量0.62~4.71 mg/g;鲜百合粉末水分、总灰分和水溶性浸出物范围分别为7.53%~10.22%、2.63%~4.88%和23.07%~43.01%。结论本研究建立的鲜百合质量控制方法准确稳定,重复性好,可用于鲜百合的质量控制。
Objective To establish the quality control method for fresh Lilium.Methods Qualitative identification of fresh Lilium was established by thin layer chromatography(TLC)method,and the content of regaloside B was determined by high performance liquid chromatrgraphy(HPLC)method.Water,total ash,and water-soluble extractives were also determined according to the Chinese Pharmacopeia(2015 Version,Volume 4).Results TLC was carried out by using silica gel G as the coating substance and petroleum ether-dichloromethane-ethyl acetate-methanol(7∶10∶7∶2)as developer.After exposing to sulfuric acid ethanol(10%),the thin layer plates were examined under ultraviolet light at 365 nm.The fresh Lilium sample showed the same color spots in the same position as the control,with clear spots and good repeatability.The HPLC was performed by Agilent C18 column(4.6 mm×250 mm,5μm),with acetonitrile-0.1%phosphoric acid(17∶83)as mobile phase,detection wavelength 312 nm,column temperature 25℃,flow rate 1.0 mL/min and injection volume 20μL.Under the condition,the linear range of regaloside B was 10.27-164.32 mg/L(R^2=0.9997),and the average recovery was 100.08%(RSD 2.31%).In 20 batches of samples,the content ranges of regaloside B,water,total ash and water-soluble extractives were 0.62-4.71 mg/g,7.53%-4.22%,2.63%-4.88%and 23.07%-43.01%,respectively.Conclusion The established quality control method of fresh Lilium is accurate,stable and repeatable,and can be used for the quality control of fresh Lilium.
作者
顾安娜
王亚茹
商云霞
唐逢雨
刘世欣
尉小慧
GU An'na;WANG Yarn;SHANG Yunxia;TANG Fengyu;LIU Shixin;WEI Xiaohui(The MOE Key Laboratory for Standardization of Chinese Medicines,Institute of Chinese Materia Medica,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China;Shanghai R&D Center for Standardization of Chinese Medicine,Shanghai 201203,China)
出处
《上海中医药杂志》
2021年第1期78-82,共5页
Shanghai Journal of Traditional Chinese Medicine
关键词
鲜百合
王百合苷B
质量标准
薄层色谱
高效液相色谱
fresh Lilium
regaloside B
quality standard
thin layer chromatography(TLC)
high performance liquid chromatrgraphy(HPLC)