[關(guān)鍵詞]
[摘要]
目的 研究右旋龍腦-β-環(huán)糊精最佳包合工藝,并對(duì)其進(jìn)行結(jié)構(gòu)表征。方法 分別采用飽和水溶液法、超聲法、研磨法對(duì)右旋龍腦進(jìn)行包合,以綜合評(píng)分為指標(biāo),篩選最佳包合方法。采用L9(34)正交試驗(yàn)設(shè)計(jì),篩選超聲法制備包合物的最佳工藝參數(shù)。采用薄層色譜(TLC)法、傅里葉紅外光譜(FIIR)法、X射線粉末衍射(XRD)法對(duì)包合物進(jìn)行結(jié)構(gòu)表征。結(jié)果 制備包合物的最佳工藝參數(shù)為:右旋龍腦與β-環(huán)糊精投料比為1∶6,超聲溫度為40 ℃,超聲時(shí)間為60 min。在該制備工藝條件下包合物的得率高于88.59%,包合率高于95.98%。經(jīng)過TLC、FIIR和XRD確證其包合物已形成。結(jié)論 本工藝具有較好的包合率和得率,右旋龍腦被β-環(huán)糊精包合后呈現(xiàn)新的物相特征。
[Key word]
[Abstract]
Objective To study the best preparation conditions of d-borneol-β-cyclodextrin inclusion complex and its structure characterization. Method The inclusion complex was prepared by the methods of saturated solution method, ultrasonic method, and grinding method with composite grade as index. To obtain the best preparation conditions of inclusion complex, L9(34) orthogonal test design was carried out. The structure of inclusion complex was identified by the methods of thin layer chromatography (TLC), Fourier infrared spectrum (FIIR) and X-ray powder diffractometry (XRD). Results The optimum preparation conditions were as follows: ratio of d-borneol and β-cyclodextrin was 1:6, ultrasound temperature was 40 ℃, ultrasound time was 60 min. The yield of inclusion complex was over 88.59%, and the inclusion ratio of inclusion complex was over 95.98% under the optimum conditions. The formation of inclusion complex was proved by TLC, FIIR, and XRD. Conclusion This technology has good inclusion rate and yield, and the d-borneol-β-cyclodextrin inclusion complex exhibits some new physical characteristics.
[中圖分類號(hào)]
[基金項(xiàng)目]
廣東省自然科學(xué)基金博士啟動(dòng)項(xiàng)目(10451064101005160);省部產(chǎn)學(xué)研結(jié)合項(xiàng)目(2009A090100041,2010B090500033);中央高?;究蒲袠I(yè)務(wù)費(fèi)專項(xiàng)資金資助項(xiàng)目(2011ZM0099)