夏桑菊颗粒氨基酸类成分指纹图谱的研究

HPLC fingerprint of amino acids compounds of Xiasangju Granules

目的:建立夏桑菊颗粒(夏枯草、野菊花、桑叶)氨基酸类成分HPLC指纹图谱。方法:采用AQC(6-氨基酸喹啉-N-羟基琥珀酰亚胺基-氨基甲酸酯)柱前衍生化HPLC法。色谱柱为SYMMETRY C18分析柱(150mm×4.6mm,5μm),流动相:(A)pH为5.05的醋酸钠缓冲液、(B)60乙腈(梯度洗脱);柱温:30℃;流速:1.0mL/min。荧光检测:激发波长(Ex)为250nm,发射波长(Em)为395nm,分析时间50min。结果:确定12个色谱峰作为共有峰,利用夹角余弦系数,相关系数及指纹图谱相似度评价系统软件,测得10批夏桑菊颗粒指纹图谱相似度0.95～1.00之间。结论:本实验建立的夏桑菊颗粒氨基酸类成分HPLC指纹图谱方法准确可靠,可控性强,重复性好,为有效控制夏桑菊颗粒质量提供可靠依据。

AIM： To establish the fingerprint chromatogram of amino acids compounds of Xiasangju Granules （ Spica Prunellae, Flos Chrysanthemi indici, Folium mori. ）. METHODS： To apply 6-aminoqtiinoly-N-hydroxy-succinimdyl carbamate （AQC） pre-column derivatization HPLC method. Separation was performed on SYMMETRY Cls（ 150 mm ×4.6 mm, 5μm） analytical column with mobile phase consisting of acetate（pH =5.05 ） and 60% acetonitrile with gradient elution with the flow rate 1.0 mL/min and the column temperature at 37℃. The Fluorescence wavelength used for detection was set at 250 nm （Excitation wavelength） and 395 nm （Emission wavelength） and the analysis time was 50 min. RESULTS ： 12 co-peaks on the HPLC fingerprints of Xiasangju Granules were indicated. The similarities were determined by the coefficients of cosine and correlation. The results of similarity analysis were 0.95 - 1.00. CONCLUSION ： Perfect fingerprints were obtained which can be used for the quality control of Xiasangju Granules.