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

作　　者：王思萌 朱田密 余婷 张伟欣 陈树和 陈科力 林爱珍 孙光军 肖文洁 WANG Simeng;ZHU Tianmi;YU Ting;ZHANG Weixin;CHEN Shuhe;CHEN Keli;LIN Aizhen;SUN Guangjun;XIAO Wenjie(School of Pharmacy,Hubei University of Chinese Medicine,Hubei Wuhan 430065,China;Hubei Provincial Hospital of Chinese Medicine,Affiliated Hospital of Hubei University of Chinese Medicine,Hubei Provincial Academy of Traditional Chinese Medicine,Hubei Wuhan 430061,China)

机构地区：[1]湖北中医药大学药学院,湖北武汉430065 [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

出　　处：《中国医院药学杂志》2024年第6期677-683,共7页Chinese Journal of Hospital Pharmacy

基　　金：第七批全国老中医药专家学术经验继承工作项目(编号:国中医药人教函[2022]76号)。

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-C_(18) (150 mm×2.1 mm,5μm)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 m L·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。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,5μm)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 0.23389,0.23389,0.14004,0.14004,0.08292,0.08292,0.05158 and 0.03472.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 

分 类 号：R943[医药卫生—药剂学] R283[医药卫生—药学]