多波长HPLC结合CCD响应面法优化大七厘散多指标含量测定方法

Optimization of the Determination Method of Multi Index Content in Daqili San by Multi Wavelength HPLC Combined with CCD Response Surface

关键词:  CCD响应面  大七厘散  多指标  含量测定  HPLC  多波长切换

Key words:  CCD-RSM  Daqili san  multi index  content determination  HPLC  multi wavelength switching

摘要:

目的 建立并优化大七厘散中多个指标性成分含量测定的方法，以提升其质量标准。方法 采用HPLC多波长切换法建立大七厘散中柚皮苷、人参皂苷Rg1、血竭素高氯酸盐、大黄素、大黄酚5个指标性成分含量测定的方法，采用Central Composite Design响应面设计（CCD-RSM），优选出含量测定最佳提取工艺，并进行验证及方法学评价。结果 大七厘散多指标含量测定最佳提取工艺为溶剂加入量40 mL，甲醇体积分数75%，超声提取时间25 min，测得样品中柚皮苷、人参皂苷Rg1、血竭素高氯酸盐、大黄素、大黄酚成分的平均含量分别为0.74，2.80，1.33，0.26，0.29 mg·g^-1，且在线性范围内峰面积与质量浓度均呈良好的线性关系，加样回收率为96.75%~100.01%，RSD为0.98%~1.94%。结论 CCD-RSM优化的大七厘散多指标含量测定提取工艺，实际值与预测值吻合度高，预测性良好，方法可行；采用HPLC多波长切换法建立的多指标含量测定方法稳定、准确可靠。

Abstract:

OBJECTIVE To establish and optimize the determination method of multi index content in Daqili San, so as to improve its quality standard. METHODS HPLC multi wavelength switching method was established to determine the content of naringin, ginsenoside Rg1, draconotin perchlorate, emodin and chrysophanol in Daqili San. By using the central composite design-response surface(CCD-RSM), the extraction process of content determination was optimized, and the verification and methodology evaluation were carried out. RESULTS The best processing conditions of multi index content in Daqili San were as follows:solvent content was 40 mL; methanol concentration was 75%; ultrasound time was 25 min. The average content of naringin, ginsenoside Rg1, draconemin perchlorate, emodin and chrysophanol were 0.74, 2.80, 1.33, 0.26, 0.29 mg·g^-1, respectively. The calibration curves were linear, the average recoveries ranged from 96.75% to 100.01%, RSD ranged from 0.98% to 1.94%. CONCLUSION By using CCD-RSM to optimize extraction process of multi index content determination in Daqili San, the actual and predicted values are highly consistent with good predictability, and the method is feasible. The multi index content determination method established by HPLC multi wavelength switching method is stable, accurate and reliable.