目的 基于质量源于设计理念优化苍术挥发油内切式匀浆法的包合工艺。方法 以包合物收得率、苍术素包合率为指标,应用失效模型与效应分析法对影响综合评分的因素进行风险评估。采用Plackett-burman design设计法对潜在关键工艺参数做进一步优化,中心复合设计试验考察交互作用。构建苍术挥发油内切式匀浆法包合工艺设计空间,对设计空间进行验证。结果 具有潜在影响的关键工艺参数为剪切转速、剪切时间、包合温度、β-环糊精用量、水用量。剪切转速、β-环糊精与挥发油质量比对综合评分影响较为显著。剪切转速对包合物收得率具有显著性影响(P<0.01),而β-环糊精与挥发油质量比对苍术素包合率有显著性影响(P<0.01)。剪切转速和β-环糊精与挥发油质量比的交互作用对包合物收得率、苍术素包合率的影响均不显著。操作空间为剪切转速4 300~4 450 r/min,β-环糊精与挥发油质量比为11∶1~12∶1,验证结果实测值和预测值接近。结论 优选的苍术挥发油内切式匀浆法包合工艺稳定可行,为苍术挥发油包合物的工业化生产提供参考。

Objective To optimize inclusion process of Atractylodis Rhizoma volatile oil based on the concept of quality by design(QbD).Methods Yield of inclusion and the inclusion rate of atractylone were taken as indicators. Risk assessments of factors that affect the comprehensive score were conduct by FMEA. PBD test was used to further optimize the selected key process parameters,and CCD test was used to investigate the interaction. The design space for inclusion process of internal homogenate method of Atractylodis Rhizoma volatile oil was established, and then was verified.Results The key process parameters with potential impact include shear speed, shear time, inclusion temperature, β-cyclodextrin dosage, and water dosage. The shear speed had a significant effect on the yield of inclusion compound(P<0.01). The mass ratio of β-cyclodextrin to volatile oil had a significant effect on the inclusion rate of atractylonin(P<0.01). The interaction between shear speed and the mass ratio of β-cyclodextrin and volatile oil had no significant effect on the yield of inclusion compound and the inclusion rate of atractylone. The operating space is 4 300 — 4 450r/min for shear speed, the mass ratio of β-cyclodextrin to volatile oil was 11:1 — 12:1, and the measured value of validation results was close to the predicted value.Conclusion The optimized internal homogenate method for inclusion of Atractylodis Rhizoma volatile oil is stable and feasible, which can provide reference for the industrial production of Atractylodis Rhizoma volatile oil inclusion compounds.

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佛山市核心技术攻关项目(1920001000378)