1.上海中医药大学中药研究所中药标准化教育部重点实验室(上海 201210)
2.上海中药标准化研究中心(上海 201210)
顾安娜,女,硕士研究生,主要从事中药质量标准的制定与修订工作
尉小慧,研究员,硕士研究生导师;E-mail:xhweixh@163.com
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顾安娜, 王亚茹, 商云霞, 等. 鲜百合的质量控制研究[J]. 上海中医药杂志, 2021,55(1):78-82.
An’na GU, Yaru WANG, Yunxia SHANG, et al. Quality control for fresh
顾安娜, 王亚茹, 商云霞, 等. 鲜百合的质量控制研究[J]. 上海中医药杂志, 2021,55(1):78-82. DOI: 10.16305/j.1007-1334.2021.2003305.
An’na GU, Yaru WANG, Yunxia SHANG, et al. Quality control for fresh
目的,2,建立鲜百合质量控制方法。,方法,2,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,2,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 C,18,色谱柱(4.6 mm×250 mm,5 μm),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20 μL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,=0.999 7),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,2,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,2,To establish the quality control method for fresh ,LiLii, Bulbus.,Methods,2,Qualitative identification of fresh ,LiLii, Bulbus 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,2,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 ,LiLii, Bulbus 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 C,18, column (4.6 mm×250 mm,5 μm), 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 20 μL. Under the condition, the linear range of regaloside B was 10.27-164.32 mg/L (,R,2,=0.999 7), 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,2,The established quality control method of fresh ,LiLii, Bulbus is accurate, stable and repeatable, and can be used for the quality control of fresh ,LiLii, Bulbus.
鲜百合王百合苷B质量标准薄层色谱高效液相色谱
fresh LiLii Bulbusregaloside Bquality standardthin layer chromatography (TLC)high performance liquid chromatrgraphy (HPLC)
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