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
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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0.74,2.80,1.33,0.26,0.29mg·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。
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 from0.98% 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.
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 from0.98% 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.
引文
[1]中国药典.一部[S].2015:495-496.
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[8]高建德,朱晓玉,宋开蓉,等.星点设计-效应面法优化果胶酶酶解提取枸杞总黄酮的工艺[J].中药材,2017,40(2):421-424.
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[10]WANG B,XU Y Y,LIN Y,et al.Simultaneous determination of seven components in Xiaopiling granule by HPLCwavelength switching combined gradient elution method[J].Chin J Mod Appl Pharm(中国现代应用药学),2017,34(4):571-574.
[2]WEN X,JIANG Y L,CHEN S Z,et al.Improvement of TLCidentification of Rheum Palmatum and Radix Angelicae Sinensis in Daqili San[J].China Pharm(中国药业),2017,26(14):7-9.
[3]CHEN H L,HU S M,CHEN J,et al.Study of the quality standards of Daqili powder[J].China J Drug Rev(中国药物评价),2015,32(2):83-86.
[4]LIAO X,QIAO L,WANG Y J.Determination of arietic acid,emodin,chrysophanol and triptolide in Shenyanning tablets by HPLC[J].Chin J Mod Appl Pharm(中国现代应用药学),2017,34(4):567-570.
[5]席珊珊,谢亚晶.HPLC法同时测定大七里散中3种成分的含量[J].黑龙江科技信息,2016(12):81.
[6]郝旭亮,张永文.中药质量标准中建立多指标含量测定品的必要性浅析[J].中国执业药师,2009,3(14):514-516.
[7]CHEN H W,ZHANG C Y,REN W G,et al.Multi-index integrated evaluation method optimizes water-extraction and ethanol precipitation of Xuanbi’antong formula(XBF)[J].China J Chin Mater Med(中国中药杂志),2016,41(1):70-74.
[8]高建德,朱晓玉,宋开蓉,等.星点设计-效应面法优化果胶酶酶解提取枸杞总黄酮的工艺[J].中药材,2017,40(2):421-424.
[9]ZHANG H Y,ZHAO M,CHEN F F,et al.Optimization of matrix formulation for Qushi Zhiyang Gel by central composite design-response surface methodology[J].JLiaoning Univ TCM(辽宁中医药大学学报),2018,20(4):154-157.
[10]WANG B,XU Y Y,LIN Y,et al.Simultaneous determination of seven components in Xiaopiling granule by HPLCwavelength switching combined gradient elution method[J].Chin J Mod Appl Pharm(中国现代应用药学),2017,34(4):571-574.
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