不同采收期老翘中化学成分含量测定

Content Determination of Chemical Compositions of Old Alice with Different Harvest Time

[目的]通过对不同采收期老翘内连翘苷、连翘酯苷A、浸出物的含量测定,为老翘适宜采收期的确定提供科学依据。[方法]采用HPLC法测定不同采收期老翘果实中连翘苷、连翘酯苷A的含量；采用《中国药典》2010版一部（附录ⅩΑ）项下醇溶性浸出物冷浸法测定；以Luna5uC18（2）100A（250 mm×4.6 mm,5μm）为色谱柱,连翘苷测定流动相为乙腈-水（25∶75,V∶V）,检测波长为277 nm,柱温为室温,流速为1.0 mL/min；连翘酯苷A测定流动相为乙腈-0.4%冰醋酸溶液（15∶85,V∶V）,检测波长为330 nm,柱温为室温,流速为1.0mL/min。[结果]连翘苷在3.33～13.32μg范围内线性关系良好（R2=0.999 7）,平均回收率为98.9%,RSD=1.8%；连翘酯苷A在4.17～6.69μg具有良好的线性关系（R2=0.999 7）,平均回收率为101.7%,RSD=0.9%。[结论]连翘苷、连翘酯苷A、浸出物在老翘整个采收期试验过程中都呈现不断下降的趋势,其中连翘苷的含量测定结果在老翘整个采收期试验过程中都达不到2010版药典的规定标准,连翘酯苷A、浸出物的含量结果分别在2013年1月20日、2月25日采集的样品测定结果中达不到2010版药典的规定标准。

[Objective] The aim was to provide a scientific basis for determination of harvest time of the old alice, through the determination of forsythin, forsythoside A and extract in old alice with different harvest time.[Method] HPLC method was used for analyzing the contents of forsythin and forsythiaside A in different harvest time of old alice, and multi-speed oscillator was used for analyzing the contents of extract. Luna5uC18（2） 100A（250 mm ×4.6 mm, 5 μm） column was carried out and the mobile phrase of determination forsythin was acetonitrile-water（25∶75, V∶V） and the detection wavelength was 277 nm.The mobile phase of determination forsythiaside A was acetonitrile-0.4% acetic acid（15∶85, V∶V）and the detection wavelength was 330 nm.The column temperature was room temperature. And the flow rate was 1.0 mL/min.[Results] There was a good linear relationship（R2=0.999 7） for forsythin at 3.33-13.32 μg and the average recovery rate was 98.9%,and RSD was 1.8%.The good linear relationship（R2=0.999 7） was for forsythiaside A at 4.17-6.69 μg and the average recovery rate was 101.7% and RSD was 0.9%. [Conclusion] Forsythin, forsythiaside A and extract were decreased during the whole experiment have shown a declining trend, in which the content of phillyrin in the whole experiment were not up to the required 2010 version Pharmacopoeia standards. Forsythiaside A and extract respectively in January 20 th, 2013 and February 25 thwould not meet the required standard Pharmacopoeia 2010 edition.