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目的:建立测定金玄痔科熏洗散(JZXS)及新工艺制备的金玄痔科熏洗散(AIG)中绿原酸、咖啡酸、金丝桃苷和木犀草素的HPLC分析方法。方法:采用Venusil XBP C18柱(250 mm×4.6 mm,5μm);柱温30℃;流速1.0mL·min-1;流动相:乙腈-0.4%磷酸水溶液,梯度洗脱;进样量10μL;检测波长为335 nm。结果:绿原酸、咖啡酸、金丝桃苷、木犀草素的线形范围分别和回归方程分别为0.760～4.560μg(r=0.999 9),Y=2 254.9 X+131.66;0.058～0.348μg(r=0.999 9),Y=3 610.8X+7.913 5;0.046～0.276μg(r=0.999 9),Y=1 446.7 X+2.124 3;0.024～0.144μg(r=0.999 9),Y=2 344.5 X-0.716 2;JZXS平均加样回收率(n=5)分别为97.4%(RSD=1.8%),98.6%(RSD=2.3%)和97.8%(RSD=2.9%);AIG平均加样回收率(n=5)为97%(RSD=1.2%),97.3%(RSD=2.5%),98.2%(RSD=2.7%)和96.9%(RSD=1.9%)。结论:该方法专属性好,准确度高,为进一步完善JZXS的质量标准提供了科学依据,并为该传统制剂二次开发为创新中药品种奠定了基础。
OBJECTIVE: To establish an HPLC method for the determination of chlorogenic acid, caffeic acid, hyperoside and luteolin in Jinxuan Hemorrhoid Washing Powder (AIG) prepared by JZXS and a new process. Methods: Venusil XBP C18 column (250 mm × 4.6 mm, 5 μm) was used. The column temperature was 30 ℃ and the flow rate was 1.0 mL · min -1. The mobile phase consisted of acetonitrile-0.4% phosphoric acid solution with gradient elution. The wavelength is 335 nm. Results: The linear ranges of chlorogenic acid, caffeic acid, hyperin and luteolin were respectively 0.760 ~ 4.560μg (r = 0.999 9), Y = 254.9X + 131.66 and 0.058 ~ 0.348μg Y = 3 610.8X + 7.913 5; 0.046-0.276 μg (r = 0.999 9), Y = 1146.7 X + 2.124 3; 0.024-0.1414 μg (r = 0.999 9), Y = 2 344.5 (RSD = 1.8%), 98.6% (RSD = 2.3%) and 97.8% (RSD = 2.9%) for the average recovery of JZXS (n = 5) The rates (n = 5) were 97% (RSD = 1.2%), 97.3% (RSD = 2.5%), 98.2% (RSD = 2.7%) and 96.9% (RSD = 1.9%). Conclusion: This method has good specificity and high accuracy, which provides a scientific basis for further improving the quality standard of JZXS, and lays the foundation for the second development of this traditional preparation for innovation of traditional Chinese medicine.