雪松松针HPLC特征图谱及6个成分的含量测定

目的:利用高效液相色谱法建立雪松松针的特征图谱,同时测定其原儿茶酸、原儿茶醛、二氢杨梅素、咖啡酸、阿魏酸、芦丁6个成分的含量。方法:采用CAPCELL PAK-C18色谱柱(250 mm×4.6 mm,5μm),以甲醇(A)-0.1%磷酸水(B)为流动相,梯度洗脱,流速为1 mL·min^-1,检测波长300 nm,柱温30℃;应用中药色谱指纹图谱相似度评价软件(2012.130723版本)对14批雪松松针进行相似度分析,同时对其6个成分的含量进行测定。结果:14批雪松松针样品的色谱图与特征图谱的相似度介于0.932~0.992之间,标定共有峰22个,并对其6个共有峰进行归属。14批样品中原儿茶酸、原儿茶醛、二氢杨梅素、咖啡酸、阿魏酸、芦丁6个成分的含量范围分别为34.312~1216.750μg·g^-1、5.246~12.533μg·g^-1、43.912~132.047μg·g^-1、50.791~145.021μg·g^-1、13.543~70.379μg·g^-1、82.763~243.758μg·g^-1,结论:所建立的HPLC特征图谱结合6个化学成分的含量测定,能较全面反映雪松松针内在化学成分质量,简便可行、快速准确,可为其质量控制提供参考。

HPLC characteristic chromatogram and assay of six components for pine needles of Cedrus deodara

Objective:To establish an HPLC characteristic chromatogram of pine needles of cedrus deodara and to develop simultaneous determination method of protocatechuic acid,protocatechuic aldehyde,dihydromyricetin,caffeic acid,ferulic acid and rutin in the sample.Methods:HPLC analysis was performed on a CAPCELL PAK-C18 column(250 mm×4.6 mm,5μm).The mobile phase consisted of methanol(A)and 0.1% phosphoric acid aqueous solution(B)with gradient elution.The flow rate was 1 mL·min^-1,the detection wavelength was 300 nm and the column temperature was 30℃.TCM chromatographic fingerprint similarity evaluation software(2012.130723 version)was used for similarity analysis in 14 batches of pine needles of Cedrus deodara,and the contents of six components in 14 batches of samples were determined at the same time.Results:The similarities between the characteristic chromatogram and chromatograms of 14 batches of pine needles in Cedrus deodara were between 0.932 and 0.992.There were altogether 22 common peaks,and six of them were identified.The contents of protocatechuic acid,protocatechuic aldehyde,dihydromyricetin,caffeic acid,ferulic acid and rutin in 14 batches of samples were in the range of 34.312^-1216.750μg·g^-1,5.246^-12.533μg·g^-1,43.912^-132.047μg·g^-1,50.791^-145.021μg·g^-1,13.543-70.379μg·g^-1 and 82.763-243.758μg·g^-1,respectively.Conclusion:The combination of the HPLC characteristic chromatogram and content determination of six components can reflect inherent quality of pine needles of Cedrus deodara.The proposed method is simple,feasible,rapid and accurate,providing reference for quality evaluation of the drug.