Université Lille Nord de France, F-59000 Lille, France.
Carbohydr Res. 2011 Oct 18;346(14):2193-9. doi: 10.1016/j.carres.2011.07.010. Epub 2011 Jul 21.
An amorphous solid of cyclomaltoheptaose (β-cyclodextrin, β-CD) was formed by milling its crystalline form using a high-energy planetary mill at room temperature. The glass transition of this amorphous solid was found to occur above the thermal degradation point of the material preventing its direct observation and thus its full characterization. The corresponding glass transition temperature (T(g)) and the ΔC(p) at T(g) have, however, been estimated by extrapolation of T(g) and ΔC(p) of closely related amorphous compounds. These compounds include methylated β-CD with different degrees of substitution and molecular alloys obtained by co-milling β-CD and methylated β-CD (DS 1.8) at different ratios. The physical characterization of the amorphous states have been performed by powder X-ray diffraction and differential scanning calorimetry, while the chemical integrity of β-CD upon milling was checked by NMR spectroscopy and mass spectrometry.
室温下，使用高能行星磨将结晶态环七葡萄糖（β-环糊精，β-CD）研磨成无定形固体。发现该无定形固体的玻璃化转变发生在材料热降解点以上，从而阻止了对其的直接观察，也阻止了对其的全面表征。然而，通过对密切相关的无定形化合物的玻璃化转变温度（T(g)）和ΔC(p)进行外推，估算出了相应的玻璃化转变温度（T(g)）和ΔC(p)。这些化合物包括具有不同取代度的甲基化 β-CD 和通过共研磨 β-CD 和甲基化 β-CD（DS 1.8）以不同比例获得的分子合金。通过粉末 X 射线衍射和差示扫描量热法对无定形态进行了物理表征，通过 NMR 光谱和质谱检查了研磨过程中 β-CD 的化学完整性。
