瓜蒌薤白正丁醇部位腺苷含量及特征图谱

目的:建立测定瓜蒌薤白正丁醇部位腺苷含量的高效液相色谱(HPLC)分析方法,并在此基础上建立正丁醇部位的特征图谱。方法:通过HPLC/PDAD联用建立瓜蒌薤白颗粒正丁醇部位特征图谱,以渐进窗口正交投影分析法进行色谱峰匹配,测定腺苷的含量;利用均值和中位数建立共有模式,采用相关系数和夹角余弦计算瓜蒌薤白颗粒正丁醇部位与共有模式间的相似程度。结果:腺苷在0.10～2.00μg范围内线性关系良好,回归方程为:Y=3100000X+2433.5,相关系数r=0.9998,平均回收率为97.34%,RSD(%)=1.14%,测定了10个批次瓜蒌薤白颗粒正丁醇部位腺苷的平均含量为0.795%;建立了瓜蒌薤白颗粒正丁醇部位HPLC特征图谱,谱间有10个共有峰,利用相关系数计算平均相似度:取均值为0.8388,取中位数为0.8245;利用夹角余弦计算平均相似度:取均值为0.8697,取中位数为0.8558。结论:瓜蒌薤白颗粒正丁醇部位中腺苷的含量测定方法的重复性及稳定性较好,同时建立了瓜蒌薤白颗粒正丁醇部位特征图谱的共有模型,可用于瓜蒌薤白颗粒正丁醇部位的质量评价。

Determination of adenosine content and characteristic spectrum of n-butanol extrac- tion in Gualou Xiebai granules

Objective：To develop an analytic protocol for the determina- tion of adenosine content of n-butanol extraction in Gualou Xiebai granules by high performance liquid chromatography （ HPLC ） , and to characterize the spectrum for n-butanol extraction on that basis. Methods ： The charac- teristic spectrum for n-butanol extraction in Gualou Xiebai granules was characterized by combined use of HPLC and PDAD, and the peaks were matched with the asymptotic window orthogonal projection analytical method to determine the adenosine content. On basis of common pattern of mean and the median, the similarity degree between n-butanol extraction in Gualou Xiebai granules was identified by calculating the correlation co- efficient method and the included angle cosine. Results： The adenosine level showed a good linear relationship at from 0.10μg to 2.00 μg. and the regression equation was：Y = 3 100 000X ＋ 2 433.5 （ r = 0. 9998 ）. Average recovery rate arrived at 97.34% （ RSD = 1.14% ）. The average content of adenosine was 0. 795% measured in 10 different batches of samples. The characteristic spectrum of n-butanol extraction in Gualou Xiebai granules was successfully established which revealed 10 common peaks in spectra. The average similarity degree estimated by correlation coefficient and included angle cosine was 0. 8388 and 0. 8697 by mean value and 0. 8245 and 0. 8558 by value of the median,respectively. Con- clusion：The protocol for determining the adenosine content of n-butanol extraction in Gualou Xiebai granules may lead to relatively better repeat- ability and stability, and successfully established characteristic spectrum for n-butanol extraction in Gualou Xiebai granules may have the implica- tion for verifying the quality of n-butanol extraction in such herbs.