短柄五加茎皮的HPLC指纹图谱研究

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.