何首乌炮制过程中5种化学成分的含量变化

目的:建立制何首乌中5种化学成分没食子酸、5-羟甲基糠醛(5-HMF)、2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷、大黄素与大黄素甲醚的含量测定方法,并比较5种成分在炮制时间变化过程中含量的动态变化.方法:采用RP-HPLC法,色谱柱为KinetexTMC18(4.6 mm×100 mm,2.6 μm);流动相为乙腈-0.5％乙酸梯度洗脱;流速为1.8 mL·min-1;柱温为30℃;检测波长分别为254,270,284,320 nm,检测时间为36 min.结果:没食子酸、5-HMF、二苯乙烯苷、大黄素与大黄素甲醚分别在0.585 ～ 58.5,0.54 ～ 53.5,1.07 ～107,1.23～123,0.564 ～ 16.92 mg·L-1线性良好.没食子酸炮制后含量明显增加,但随着炮制时间延长其含量变化不大;5-HMF为炮制后新产生的成分,其含量随着炮制时间的延长而有所增加;二苯乙烯苷随着炮制时间的延长,其含量呈下降趋势;游离蒽醌类物质大黄素与大黄素甲醚,两者炮制后均比炮制前要高,而且都在炮制后32 h达最高峰.结论:提供了一种结果准确、重复性好、快捷的(制)何首乌质量分析方法.何首乌炮制过程中化学成分变化与其药效之间的相关性及量效关系有待进一步深入的研究.

Content Changes of 5 Components in Polygohum muhiflorum During Processing

Objective:To study the content changes of gallic acid,5-hydroxymethyl furfural,emodin,2,3,5,4’-tetrahydroxystilbene-2-O-β-D-glucoside and emodin monomethyl ether in Polygohum muhiflorum during processing and establish a method of determination by HPLC.Method: The separation was performed on a KinetexTM C18 column(4.6 mm×100 mm,2.6 μm),using acetonitrile and water(0.5% acetic acid pH 2.9)as the mobile phase with gradient elution.The flow rate was 1.8 mL·min-1;column temperature was at 30 ℃ and the detection wavelength was 254,270,284,320 nm,respectively.Result: The linear ranges of gallic acid,5-hydroxymethylfurfural,emodin,2,3,5,4’-tetrahydroxystilbene-2-O-β-D-glucoside and emodin monomethyl ether were 0.585-58.5,0.54-53.5,1.07-107,1.23-123,0.564-16.92 mg·L-1,respectively.The content of gallic acid was increased significantly and 5-HMF was a new component after processing,and timing had a little effect on the content change of gallic acid,however,the content change of 5-HMF was higher and higher in the process of time till 72 h.Meanwhile,the content of stilbene glycoside was decreased in the process of time during processing and dissociative anthraquinone,emodin and emodin monomethyl ether,both of them were increased by processing after 32 h the content reach the maximum.Conclusion: The method is simple,accurate and can be used for quality control of P.muhiflorum.Further research of the correlation between the content changes of these 5 components in P.muhiflorum and pharmacodynamics as well as dose-effect relationship should be done.