目的 基于質(zhì)量源于設計理念優(yōu)化蒼術揮發(fā)油內(nèi)切式勻漿法的包合工藝。方法 以包合物收得率、蒼術素包合率為指標,應用失效模型與效應分析法對影響綜合評分的因素進行風險評估。采用Plackett-burman design設計法對潛在關鍵工藝參數(shù)做進一步優(yōu)化,中心復合設計試驗考察交互作用。構建蒼術揮發(fā)油內(nèi)切式勻漿法包合工藝設計空間,對設計空間進行驗證。結果 具有潛在影響的關鍵工藝參數(shù)為剪切轉(zhuǎn)速、剪切時間、包合溫度、β-環(huán)糊精用量、水用量。剪切轉(zhuǎn)速、β-環(huán)糊精與揮發(fā)油質(zhì)量比對綜合評分影響較為顯著。剪切轉(zhuǎn)速對包合物收得率具有顯著性影響(P<0.01),而β-環(huán)糊精與揮發(fā)油質(zhì)量比對蒼術素包合率有顯著性影響(P<0.01)。剪切轉(zhuǎn)速和β-環(huán)糊精與揮發(fā)油質(zhì)量比的交互作用對包合物收得率、蒼術素包合率的影響均不顯著。操作空間為剪切轉(zhuǎn)速4 300~4 450 r/min,β-環(huán)糊精與揮發(fā)油質(zhì)量比為11∶1~12∶1,驗證結果實測值和預測值接近。結論 優(yōu)選的蒼術揮發(fā)油內(nèi)切式勻漿法包合工藝穩(wěn)定可行,為蒼術揮發(fā)油包合物的工業(yè)化生產(chǎn)提供參考。

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.

R282

佛山市核心技術攻關項目(1920001000378)