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目的:优化和提高大自然五花饮的质量标准。方法:采用薄层色谱(TLC)法对制剂中的菊花、甘草和木棉花进行定性鉴别。采用高效液相色谱法分别测定制剂中绿原酸和射干苷的含量:色谱柱为Diamonsil C18,流动相为乙腈-0.4%磷酸(用三乙胺调pH至2.05)(10 ∶ 90,V/V,绿原酸)或乙腈-0.4%磷酸(用三乙胺调pH至2.05)(18 ∶ 82,V/V,射干苷),流速为1 ml/min,检测波长为327 nm(绿原酸)或265 nm(射干苷),柱温为25 ℃,进样量为10 μl。结果:菊花、甘草、木棉花的TLC图斑点清晰,分离度好。绿原酸、射干苷检测质量浓度线性范围分别为19.7~98.7(r=0.999 5)、25.4~126.8 μg/ml(r=0.999 8);精密度、稳定性、重复性的RSD<4%;加样回收率分别为97.01%~104.98%(RSD=3.64%,n=9)、98.44%~104.58%(RSD=1.84%,n=9)。结论:优化和提高的标准有利于大自然五花饮的质量控制。
OBJECTIVE:To optimize and improve the quality standards of Daziran wuhua yin. METHODS: TLC was used for the qualitative identification of Cichorii Herba, Glycyrrhizae Radix et Rhizoma and Gossampinus malabarica. HPLC was used for the contents determination of chlorogenic acid and tectoridin. The column was Diamonsil C18 with mobile phase of acetonitrile -0.4% phosphoric acid (pH adjusted with to 2.05 with triethylamine) (10 ∶ 90,V/V, chlorogenic acid or 18 ∶ 82,V/V, tectoridin) at a flow rate of 1 ml/min, the detection wavelength was 327 nm (chlorogenic acid) or 265 nm (tectoridin), the column temperature was 25 ℃,and the injection volume was 10 μl. RESULTS: TLC of Cichorii Herba, Glycyrrhizae Radix et Rhizoma and G. malabarica showed clear spots and good separation. The linear range was 19.7-98.7 μg/ml for chlorogenic acid (r=0.999 5) and 25.4-126.8 μg/ml for tectoridin(r=0.999 8); RSDs of precision, stability and reprosucibility tests were lower than 4%,average recoveries were 97.01%-104.98%(RSD=3.64%,n=9)、98.44%-104.58%(RSD=1.84%,n=9). CONCLUSIONS: The optimized and improved standard is helpful for the quality control of Daziran wuhua yin.
大自然五花饮射干苷绿原酸薄层色谱法高效液相色谱法
Daziran wuhua yinTectoridinChlorogenic acidTLCHPLC
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