短柄五加茎皮的HPLC指纹图谱研究

Studies on the HPLC fingerprints of Acanthopanax brachypus bark

目的：建立短柄五加茎皮的HPLC指纹图谱及紫丁香苷含量的测定方法。方法：采用岛津C18（4.6 mm×250 mm，5 μm）色谱柱，流动相为0.15%醋酸-水（A）和0.15%醋酸-乙腈（B），进行梯度洗脱[0-10 min,A-B（9：1）；10-50 min，A-B（6：4）；50-110 min，A-B（1：9）]，流速0.8 mL·min^-1，检测波长266 nm，柱温25 ℃，进样量10 μL，分析时间为100 min。结果：在0.02-0.32 mg·mL^-1范围内，紫丁香苷的浓度与峰面积呈线性关系（r=0.9998），不同产地短柄五加茎皮中紫丁香苷的含量有一定的差别（0.22-0.41 mg·g-1）。通过对10批次短柄五加茎皮的指纹图谱进行评价，确定了16个共有色谱峰，并初步确认9-12号峰分别为绿原酸、紫丁香苷、acantrifoside A和异秦皮啶的色谱峰。结论：本研究方法具有较好的精密度、重复性和稳定性，从整体上显示了短柄五加茎皮的化学特征，为短柄五加药材的质量评价和控制提供了有效手段。

Objective： To establish the HPLC fingerprint and the determination method of the content of syringin in the barks of Acanthopanax brachypus. Methods： HPLC was performed on a Shimadzu C18 column（4.6 mm×250 mm,5 μm）at the column temperature of 25 ℃.The mobile phase consisted of 0.15%acetic acid（A） and 0.15%acetonitrile（B） with a gradient elution [0-10 min,A-B（9：1）,10-50 min,A-B（6：4）,50-110 min,A-B（1：9）].The flow rate was 0.8 mL·min^-1,the detection wavelength was 266 nm,the sample volume was 10 μL and the analysis time was 100 min. Results： With the HPLC method,the calibration curve for the concentration and peak area of syringin had good linear relationship in the range of 0.02-0.32 mg·mL^-1 with the correlation coefficient of 0.9998.There was difference in the content of syringin among Acanthopanax brachypus of different producing areas（0.22-0.41 mg·g-1）.The HPLC fingerprints of 10 batches of Acanthopanax brachypus barks were evaluated and 16 common chromatographic peaks were marked.No.9-12 peaks were identified to be chlorogenic acid,syringin,acantrifoside A and isofraxidin,respectively. Conclusion： This method is accurate and steady with a good precision and reproducibility,showing the overall chemical characteristics of Acanthopanax brachypus bark,providing an effective means for the quality evaluation and control of Acanthopanax brachypus.