论文部分内容阅读
目的:建立黄柏及黄柏炭饮片的HPLC特征图谱,分析黄柏饮片炒炭前后特征图谱的变化规律。方法:采用HPLC分析黄柏及黄柏炭饮片的特征图谱,色谱条件为ZORBAX SB-C18色谱柱(4.6 mm×250 mm,5μm),流动相乙腈(A)-0.05 mol·L~(-1)磷酸二氢钾溶液(B)(磷酸调p H 3.4)梯度洗脱(0~5 min,5%~10%A;5~20 min,10%~14%A;20~50 min,14%~32%A;50~80 min,32%~70%A),检测波长215 nm,柱温35℃,流速1.0 m L·min~(-1),进样量10μL。结果:11批黄柏饮片中均标示出16个特征峰,并归属了其中的9个色谱峰,分别为绿原酸、隐绿原酸、盐酸黄柏碱、木兰花碱、盐酸药根碱、盐酸巴马汀、盐酸小檗碱、黄柏内酯、黄柏酮。通过对色谱峰的分析,黄柏炭仅能检出黄柏中的3个共有峰,且峰面积相差较大;另外标示出了2个特征峰,其中相对比例较高的特征峰经分析验证,确认其为盐酸小檗碱的加热分解产物——小檗红碱。结论:黄柏饮片炒炭前后的特征图谱存在显著差异。该方法准确可靠、重复性好,为黄柏和黄柏炭饮片的质量标准制定提供参考依据。
OBJECTIVE: To establish HPLC profiles of Cortex Phellodendri and Cortex Phellodendri Cork Pieces, and to analyze the changes of the characteristics of Cortex Phellodendri cv. Methods: The chromatograms of Cortex Phellodendri and Cortex Phellodendri were analyzed by HPLC. The chromatographic conditions were ZORBAX SB-C18 column (4.6 mm × 250 mm, 5 μm), mobile phase of acetonitrile-0.05 mol·L -1 phosphoric acid (0 to 5 min, 5% to 10% A; 5 to 20 min, 10% to 14% A; 20 to 50 min, 14% to 5% 32% A; 50-80 min, 32% -70% A). The detection wavelength was set at 215 nm and the column temperature was 35 ℃. The flow rate was 1.0 m L · min -1. Results: Sixteen characteristic peaks were identified in 11 batches of Phellodendron chinense, and nine of them were assigned to them. They were chlorogenic acid, cryptocarcinoma acid, cork base, magnolol, jatrorrhizine hydrochloride, hydrochloric acid Palmatine, berberine hydrochloride, corticosterone, flavone. Through the analysis of chromatographic peaks, Cork charcoal can only detect the three common peaks in Phellodendron, and the peak area difference between the larger; also marked two characteristic peaks, of which the relative proportion of the higher peak was analyzed and confirmed that It is berberine hydrochloride thermal decomposition products - berberine. Conclusion: There is a significant difference in the characteristic map of Phellodendron chinense before and after the fried carbon. The method is accurate and reliable with good repeatability and provides a reference for the quality standard of Cork and Phellodendron cork.