目的 基于質(zhì)量源于設(shè)計理念優(yōu)化蒼術(shù)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(shù)素包合率為指標(biāo),應(yīng)用失效模型與效應(yīng)分析法對影響綜合評分的因素進(jìn)行風(fēng)險評估。采用Plackett-burman design設(shè)計法對潛在關(guān)鍵工藝參數(shù)做進(jìn)一步優(yōu)化,中心復(fù)合設(shè)計試驗考察交互作用。構(gòu)建蒼術(shù)揮發(fā)油內(nèi)切式勻漿法包合工藝設(shè)計空間,對設(shè)計空間進(jìn)行驗證。結(jié)果 具有潛在影響的關(guān)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(shù)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(shù)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(jié)果實測值和預(yù)測值接近。結(jié)論 優(yōu)選的蒼術(shù)揮發(fā)油內(nèi)切式勻漿法包合工藝穩(wěn)定可行,為蒼術(shù)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(shù)攻關(guān)項目(1920001000378)