多指标综合评分法结合正交试验优选温阳通便汤的水煎煮工艺
Optimization of water extraction process for Wenyang Tongbian Decoction by multi-index comprehensive scoring method plus orthogonal experiment
王思萌 1朱田密 2余婷 1张伟欣 1陈树和 2陈科力 3林爱珍 2孙光军 2肖文洁2
作者信息
- 1. 湖北中医药大学药学院,湖北武汉 430065;湖北省中医院,湖北中医药大学附属医院,湖北省中医药研究院,湖北武汉 430061
- 2. 湖北省中医院,湖北中医药大学附属医院,湖北省中医药研究院,湖北武汉 430061
- 3. 湖北中医药大学药学院,湖北武汉 430065
- 折叠
摘要
目的:优选温阳通便汤的水煎煮工艺,为该制剂的工业化生产提供参考.方法:采用液相色谱-串联三重四级杆质谱法,选择Agilent ZORBAX SB-C18(150 mm×2.1 mm,5 μm)色谱柱,流动相为乙腈(A)-0.1％甲酸溶液(B),梯度洗脱,流速为0.25 mL·min-1,柱温为30 ℃;运用多反应监测(multiple reaction monitoring,MRM)的正、负离子模式测定温阳通便汤水煎液中7种指标性成分松果菊苷、桂皮醛、毛蕊异黄酮葡萄糖苷、β-蜕皮甾酮、藁本内酯、辛弗林、异阿魏酸的含量,以7种成分含量及出膏率作为评价指标,利用层次分析法确定各评价指标的权重系数并计算综合评分.通过单因素试验考察料液比、煎煮时间、煎煮次数对综合评分的影响,确定各因素的水平.采用多指标综合评分法,以上述8个指标的综合评分为指标,设计正交试验优选温阳通便汤的水煎煮工艺参数并进行验证.结果:松果菊苷、桂皮醛、毛蕊异黄酮葡萄糖苷、β-蜕皮甾酮、藁本内酯、辛弗林、异阿魏酸及出膏率的权重系数分别为 0.233 89,0.233 89,0.140 04,0.140 04,0.082 92,0.082 92,0.051 58,0.034 72.最终优选出的温阳通便汤的水煎煮工艺为料液比1∶10,煎煮3次,每次0.5 h.3批验证试验综合评分值的RSD为6.57％.结论:该研究优选的温阳通便汤的水煎煮工艺稳定、可行.
Abstract
OBJECTIVE To optimize the water extraction process of Wenyang Tongbian Decoction(WTD)and provide ref-erences for industrial production of this preparation.METHODS Using liquid chromatography tandem triple quadrupole mass spectrometry,Agilent ZORBAX SB-C18(150 mm×2.1 mm,5 pm)was selected with a mobile phase of acetonitrile(A)and 0.1％formic acid solution(B)and a gradient elution at a flow rate of 0.25 mL·min-1.Column temperature was at 30 ℃.The positive and negative ion modes of multiple reaction monitoring(MRM)were utilized for determining the contents of 7 compo-nents,namely echinacoside,cinnamaldehyde,calycosin-7-O-β-D-glucopyranoside,β-ecdysterone,ligustilide,synephrine and isoferulic acid in the preparation of WTD.The contents and yields of 7 components were employed as evaluation parameters,weight coefficients of each parameter determined by analytic hierarchy process and comprehensive scores calculated.The effects of solid-liquid ratio,extraction time and extraction frequency on comprehensive score were examined by single factor test.The level of each factor was determined.Using comprehensive scores of the above 8 parameters,water extraction process of WTD was opti-mized by orthogonal experiment and validation tests.RESULTS Weight coefficients for the contents of echinacoside,cinnamal-dehyde,calycosin-7-O-β-D-glucopyranoside,β-ecdysterone,ligustilide,synephrine,isoferulic acid and yield of dry extract were 0.233 89,0.233 89,0.140 04,0.140 04,0.082 92,0.082 92,0.051 58 and 0.034 72.Optimal process of water extraction was determined as a solid-liquid ratio of 1∶10,extracting thrice and for 0.5 h each time.RSD of comprehensive scores of 3 batches of validation tests were 6.57％.CONCLUSION The optimized process of water extraction is both stable and feasible for WTD.
关键词
温阳通便汤/煎煮工艺/多反应监测/层次分析法/正交试验/松果菊苷/桂皮醛/β-蜕皮甾酮Key words
Wenyang Tongbian Decoction/water extraction process/multiple reaction monitoring/analytic hierarchy/orthogonal experiment/echinacoside/cinnamaldehyde/β-ecdysterone引用本文复制引用
基金项目
全国老中医药专家学术经验继承工作项目(第七批)(国中医药人教函[2022]76号)
出版年
2024
NETL
NSTL
万方数据