Manipulating the size, the morphology and the polymorphism of acetaminophen using supercritical antisolvent (SAS) precipitation

Manipulating the size, the morphology and the polymorphism of acetaminophen using supercritical antisolvent (SAS) precipitation
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DOI:
10.1016/j.supflu.2013.07.015
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发表时间:
2013-10-01
影响因子:
3.9
通讯作者:
Schluecker, Eberhard
Schluecker, Eberhard
中科院分区:
工程技术2区
文献类型:
--
作者:
Rossmann, Matthias;Braeuer, Andreas;Schluecker, Eberhard

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超临界抗溶剂技术用于结晶扑热息痛颗粒。超临界二氧化碳(scCO(2))用作抗溶剂。使用乙醇、丙酮以及乙醇和丙酮的混合物作为溶剂。对乙酰氨基酚在溶液中的初始浓度在1和5wt%之间变化,乙醇/丙酮溶剂混合物的组成在50和90wt%之间,并且在313 K的温度下操作压力在10和16 MPa之间。最重要的发现是可以通过改变溶液中乙醇的含量在单斜晶和正交晶之间调节对乙酰氨基酚晶体的多晶型。第二个重要的发现是,初级和二级晶体结构的发生可以单独解释的结晶过程中的整体过饱和度。虽然X射线衍射用于分析颗粒的多晶型物,但使用扫描电子显微镜分析它们的形态。(C)2013爱思唯尔有限公司版权所有。
The supercritical antisolvent technology is used to crystallize paracetamol particles. Supercritical carbon dioxide (scCO(2)) is used as antisolvent. Ethanol, acetone and mixtures of ethanol and acetone are used as solvents. The initial concentration of paracetamol in the solution was varied between 1 and 5 wt%, the composition of the ethanol/acetone solvent mixture between 50 and 90 wt% of ethanol and the operation pressure between 10 and 16 MPa at a temperature of 313 K. The most important finding is that the polymorph of paracetamol crystals can be adjusted between monoclinic and orthorhombic by varying the content of ethanol in the solution. The second important finding is that the occurrence of primary and secondary crystal structures can be explained solely by the overall supersaturation during the crystallization process. While X-ray diffraction was used to analyze the polymorph of the particles, their morphology was analyzed using scanning electron microscopy. (C) 2013 Elsevier B.V. All rights reserved.