超高效合相色谱法定性与定量分析补肾健脑颗粒  

Qualitative and Quantitative Analysis of Bushen Jiannao Grains by Ultra Performance Convergence Chromatography

作　　者：朱瑞娟[1] 王波 胡芳[1] 李灿[1] 柳小亚 封士兰[1] 周围 

机构地区：[1]兰州大学药学院,兰州730000 [2]甘肃出入境检验检疫局综合技术中心,兰州730000

出　　处：《分析化学》2015年第2期288-293,共6页Chinese Journal of Analytical Chemistry

基　　金：兰州市科技三项经费项目(No.2012-2-70)资助

摘　　要：用超高效合相色谱法(Ultra performance convergence chromatography,UPC2)建立补肾健脑颗粒及各药材提取物的指纹图谱,对补肾健脑颗粒主要色谱峰进行归属分析,并测定有效成分β-蜕皮甾酮和松果菊苷的含量。样品经乙醇提取后,进样1μL,用Waters ACQUITY UPC2TMBEH柱(100 mm×3.0 mm,1.7μm)分离,柱温为40℃,以超临界CO2-0.05%H3PO4-甲醇溶液为流动相,梯度洗脱,流速为0.8 m L/min。分析补肾健脑颗粒和各药材提取物的UPC2指纹图谱,利用各峰相对保留时间、紫外光谱图及部分对照品归属主峰。结果表明,补肾健脑颗粒UPC2指纹图谱中15个主峰来源明确,其中12号峰为β-蜕皮甾酮,含量为380μg/g,15号峰为松果菊苷,含量为9.562 mg/g。与HPLC和UPLC法相比,本方法简便、快速,精密度高,重现性好。An ultra performance convergence chromatographic （ UPC2 ） method was established for the attribution analysis of the main peaks as well as the quantitative determination of echinacoside andβ-ecdyserone in Bushen Jiannao Grains. The samples were extracted with ethanol and separated on Waters ACQUITY UPC2TM BEH column （100 mm × 3. 00 mm, 1. 7 μm）, with a gradient supercritical CO2-0. 05%phosphoric acid-methanol solvent system at 40 ℃. The flow rate was 0. 8 mL/min, the detection wavelength was set at 248 nm and the injection volume was 1 μL. Results showed that all the main peaks in the fingerprint were clearly attributed. The peak named 12 wasβ-ecdyserone with the content of 380μg/g and the peak named 15 was echinacoside with the content of 9. 562 mg/g. The method was simple, eco-friendly, accurate and reliable compared with HPLC and UPLC.

关 键 词：超高效合相色谱 补肾健脑颗粒 β-蜕皮甾酮 松果菊苷 

分 类 号：TQ460.72[医药卫生—药物分析学] O657.72[化学工程—制药化工]