摘要
目的采用多指标加权综合评分法优选百解合剂的提取工艺,为该制剂的研发和生产提供参考。方法采用超高效液相色谱串联三重四级杆质谱法(UPLC-MS/MS)同时测定百解合剂提取液中13种指标性成分柴胡皂苷A、柴胡皂苷D、黄芩苷、芍药苷、(-)-丁香树脂酚-4-O-β-D-呋喃芹糖基-(1→2)-β-D-吡喃葡萄糖苷、斯皮诺素、酸枣仁皂苷A、迷迭香酸、厚朴酚、和厚朴酚、甘草苷、甘草酸、6-姜辣素的含量,采用Waters CORTECS C18色谱柱(2.1 mm×100 mm,1.6μm),流动相为乙腈-0.1%甲酸水,梯度洗脱,流速为0.25 mL/min,柱温45℃,电喷雾正负离子切换多反应监测模式。在单因素试验基础上,采用正交试验设计,以13种成分提取量和全方得膏率为评价指标,考察加水量、提取时间、提取次数对提取效果的影响,并通过加权综合评分法优选百解合剂的提取工艺。结果最佳提取工艺参数为加10倍量水浸泡2 h,提取2次,每次2.5 h,13种成分在相应浓度范围内线性关系良好(r>0.9977),平均加样回收率为98.19%~102.39%,RSD≤3.3%。结论本研究优选的提取工艺稳定可行,可为百解合剂进一步开发利用提供依据。
Objective To optimize the extraction process of Baijie Mixture using multi-index weighted comprehensive scoring method;To provide reference for the development and production of the preparation.Methods An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was used to determine 13 indicative components(including saikosaponin A,saikosaponin D,baicalin,paeoniflorin,(-)-syringaresnol-4-O-β-D-apiofuranosyl-(1→2)-β-D-glucopyranoside,spinosin,jujubosid A,rosmarinic acid,magnolol,honokiol,liquiritin,glycyrrhizin,6-Gingerol)in the Baijie Mixture simultaneously.Chromatographic separation was achieved on Waters CORTECS C18 column(2.1 mm×100 mm,1.6μm).The mobile phase was acetonitrile(A)-0.1%formic acid water(B)with gradient elution;the flowing was set at 0.25 mL/min;the column temperature was 45℃.Multiple reaction monitoring(MRM)was adopted in positive and negtive ion switching mode.On the basis of single factor test,orthogonal test was used to investigate the influence of water amount,extraction time and extraction times on the extraction effect,and the extraction process of Baijie Mixture was optimized by weighted comprehensive scoring method,taking the extraction amount of 13 components and extraction rate of the whole recipe as evaluation indexes.Results The optimal extraction parameters were as follows:the medicinal materials were soaked in 10 times of water for 2 hours,extracted twice,2.5 hours each time.13constituents showed good linear relationships within their testing ranges(r>0.9977),and the average recoveries were98.19%–102.39%,with the RSD≤3.3%.Conclusion The optimized extraction process in the study is stable and feasible,which can provide experimental basis for further development and utilization of the Baijie Mixture.
作者
郑文炜
沈洋
许舒瑜
林锦德
褚克丹
许文
徐伟
ZHENG Wenwei;SHEN Yang;XU Shuyu;LIN Jinde;CHU Kedan;XU Wen;XU Wei(Centre of Biomedical Research&Development,Fujian University of Traditional Chinese Medicine,Fuzhou 350122,China;College of Pharmacy,Fujian University of Traditional Chinese Medicine,Fuzhou 350122,China;900th Hospital of the Joint Logistics Support Force of the Chinese People’s Liberation Arm,Fuzhou 350002,China;Anxi Hospital of Traditional Chinese Medicine,Anxi 362400,China)
出处
《中国中医药信息杂志》
CAS
CSCD
2023年第1期128-134,共7页
Chinese Journal of Information on Traditional Chinese Medicine
基金
国家自然科学基金(81503204)
福建省卫生计生科研人才培养项目(2018-ZQN-65)。
