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首页> 外文期刊>Crystal growth & design >In situ X-ray diffraction study of the crystallization of spray-dried lactose
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In situ X-ray diffraction study of the crystallization of spray-dried lactose

机译：喷雾干燥乳糖结晶的原位X射线衍射研究

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摘要

An in situ technique with X-ray diffraction analysis has been developed to study the crystallization of lactose in humid air. This technique was used in association with ex situ scanning electron microscopy to determine changes in phase composition and morphology during crystallization. Individual spherical particles of spray-dried lactose plasticize and coalesce upon absorption of moisture. Following an induction period, crystallization is rapid with the appearance of the anhydrous 5:3 phase containing both a and isomers of lactose, alpha-lactose monohydrate and beta-lactose, almost simultaneously. The 5:3 phase decomposed as the other two phases developed. After extended exposure to humid air, only alpha-lactose monohydrate and beta-lactose were observed. The predominant particle habit observed in the fully crystallized lactose is platelet. These observations are rationalized in terms of the restricted molecular diffusion in plasticized lactose preventing movement of the beta-lactose isomer toward developing alpha-lactose monohydrate crystals with the result that normal solution phase inhibition of growth of the (0 (1) over bar1) face leading the tomahawk shaped crystal lactose does not occur. The restricted diffusional conditions also favor the formation of the mixed isomer 5:3 phase, resulting in the entrapment of both isomers during crystallization.
机译：已经开发出一种具有X射线衍射分析的原位技术来研究潮湿空气中乳糖的结晶。将该技术与异位扫描电子显微镜结合使用，以确定结晶过程中相组成和形态的变化。喷雾干燥乳糖的单个球形颗粒在吸收水分后会增塑并聚结。诱导期后，结晶迅速发生，几乎同时出现包含乳糖的α和异构体，α-乳糖一水合物和β-乳糖的无水5：3相。 5：3阶段随着其他两个阶段的发展而分解。长时间暴露于潮湿空气后，仅观察到α-乳糖一水合物和β-乳糖。在完全结晶的乳糖中观察到的主要颗粒习性是血小板。根据增塑乳糖中的受限分子扩散来阻止β-乳糖异构体向发展中的α-乳糖一水合物晶体移动，这些观察是合理的，其结果是正常溶液相抑制了（0（1）在bar1）面上的生长导致不会出现战斧形的结晶乳糖。受限的扩散条件也有利于混合异构体5：3相的形成，导致两种异构体在结晶过程中截留。

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