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目的:比较不同来源的β-环糊精(β-CD)对薄荷脑的包合率。方法:采用研磨法制备β-环糊精-薄荷脑包合物,通过TLC法、粉末X射线衍射法和GC法对包合物进行鉴定和表征。粉末X射线衍射分析条件:Cu Kα辐射石墨单色器;管压为40k V,管流为40 m A;扫描范围为3~35°;扫描步长为0.02°,扫描速率为5°·min~(-1)。GC色谱条件:采用Agilent DB-wax毛细管色谱柱(30 m×0.53 mm,1.0μm),柱温为120℃,进样口温度为250℃,采用火焰离子化检测器(FID),检测器温度为250℃;分流比为10∶1。结果:TLC和粉末X射线衍射试验均证明包合物的形成。进口和国产β-CD对薄荷脑的包合率分别为47.9%和25.0%。结论:本试验所采用的方法简便、快速、准确,可用于测定不同来源β-CD对薄荷脑的包合能力。结果表明进口β-CD的包合效果优于国产β-CD。
Objective: To compare the inclusion rates of β-cyclodextrin (β-CD) to menthol in different sources. Methods: β-Cyclodextrin-menthol inclusion complex was prepared by grinding method. The inclusion complex was identified and characterized by TLC, powder X-ray diffraction and GC. Conditions of powder X-ray diffraction analysis: Cu Kα radiation graphite monochromator; tube pressure 40 kV, tube flow 40 m A; scanning range 3 to 35 °; scanning step 0.02 °; scanning rate 5 ° · min ~ (-1). GC Chromatographic conditions: An Agilent DB-wax capillary column (30 m × 0.53 mm, 1.0 μm) was used with a column temperature of 120 ° C and an inlet temperature of 250 ° C using a flame ionization detector (FID) 250 ° C; split ratio 10: 1. Results: Both TLC and powder X-ray diffraction proved the formation of inclusion complex. The inclusion rates of imported and domestic β-CD to menthol were 47.9% and 25.0% respectively. Conclusion: The method used in this study is simple, rapid and accurate and can be used to determine the inclusion of different sources of β-CD on menthol. The results showed that the inclusion β-CD import better than domestic β-CD.