羌藿祛湿清瘟颗粒挥发油β-环糊精包合物的制备、表征及定量分析
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篇名: 羌藿祛湿清瘟颗粒挥发油β-环糊精包合物的制备、表征及定量分析
TITLE: Preparation,characterization and quantitative analysis of β-cyclodextrin inclusion complex with volatile oil from Qianghuo qushi qingwen granules
摘要: 目的 制备羌藿祛湿清瘟颗粒挥发油β-环糊精(β-CD)包合物,对其进行表征及定量分析。方法以包合率、包合物收得率计算的综合评分为指标,筛选包合方法;以上述综合评分为响应值,以β-CD与挥发油比例、包合温度、包合时间为考察指标,采用单因素实验和Box-Behnken响应面实验优化包合工艺条件并验证;按最优包合工艺制备羌藿祛湿清瘟颗粒挥发油包合物,进行紫外-可见光谱扫描、薄层色谱分析、显微成像观察,并采用超高效液相色谱法测定包合物中紫苏醛、广藿香酮、苍术素的含量。结果包合方法采用饱和水溶液法,最优包合工艺条件为β-CD与挥发油比例7.5∶1、包合温度40℃、包合时间2.2h;3次验证实验所得包合率均值为72.32%,包合物收得率均值为74.45%,综合评分均值为72.96分,与模型预测值(74.15分)的相对误差为1.61%。紫外-可见光谱扫描、薄层色谱分析、显微成像观察显示,β-CD已与挥发油成功形成新的包合物;包合物中紫苏醛、广藿香酮、苍术素的平均含量分别为4.4982、0.8149、0.9057mg/g(RSD分别为0.31%、0.56%、0.63%,n=3)。结论成功建立了稳定、可行的羌藿祛湿清瘟颗粒挥发油包合物制备工艺。
ABSTRACT: OBJECTIVE To prepare the β -cyclodextrin ( β -CD) inclusion complex with volatile oil from Qianghuo qushi qingwen granules, and to characterize and quantitatively analyze the inclusion complex. METHODS The comprehensive scores calculated by inclusion rate and inclusion compound yield were used as indicators for screening the inclusion method. The single-factor experiments and Box-Behnken response surface experiments were used to op timize the inclusion conditions, with the above comprehensive score as response value, and taking the ratio of β -CD to volatile oil, inclusion temperature and inclusion time as indexes. The volatile oil inclusion complex of Qianghuo qushi qingwen granules was prepared according to the determined optimal process, followed by validation. Ultraviolet (UV)-visible spectroscopy, thin-layer chromatography (TLC), and microscopic imaging were also performed. Ultra-high performance liquid chromatography was used to determine the contents of perillaldehyde, pogostone and atractylodin. RESULTS The saturation aqueous solution method was adopted. The optimal inclusion process conditions were as follows: the ratio of β -CD to volatile oil was 7.5∶1, the inclusion temperature was 40 ℃, and the inclusion time was 2.2 h. In three verification experiments, the average inclusion rate was 72.32%, the average yield of inclusion compound was 74.45%, the average comprehensive score was 72.96 points, and the relative error with the predicted value (74.15 points) of the model was 1.61%. UV-visible spectroscopy, TLC and microscopic imaging showed that β -CD and volatile oil successfully formed a new inclusion complex. The average contents of perillaldehyde, pogostone and atractylodin were 4.498 2, 0.814 9, 0.905 7 mg/g, respectively, with RSDs of 0.31%, 0.56% and 0.63% ( n =3). CONCLUSIONS A stable and feasible preparation process of the volatile oil inclusion complex of Qianghuo qushi qingwen granules is successfully established.
期刊: 2026年第37卷第06期
作者: 孙奕成;覃翎瑞;邹恺平;赵晨光;窦莉;刘顺;赵林钢
AUTHORS: SUN Yicheng,QIN Lingrui,ZOU Kaiping,ZHAO Chenguang,DOU Li,LIU Shun,ZHAO Lingang
关键字: 羌藿祛湿清瘟颗粒;挥发油;包合工艺;Box-Behnken响应面实验;表征;定量分析
KEYWORDS: Qianghuo qushi qingwen granules; volatile oil; inclusion process; Box-Behnken response surface experiment;
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