Toward Phase Quantification at the Nanoscale Using the Total Scattering Pair Distribution Function (TSPDF) Method: Recrystallization of Cryomilled Sulfamerazine
Toward Phase Quantification at the Nanoscale Using the Total Scattering Pair Distribution Function (TSPDF) Method: Recrystallization of Cryomilled Sulfamerazine
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使用总散射对分布函数 (TSPDF) 方法进行纳米级相定量：冷冻研磨磺胺嘧啶的重结晶
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发表时间：
2013
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通讯作者：
S. Billinge
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作者：
Timur Davis;Matthew N. R. Johnson;S. Billinge
制药行业面临的最具挑战性的问题之一是识别和量化混合相样品中含有结晶，纳米晶和非晶组分的相分数。在这里，我们证明了一种方法，实现这一点，使用高能X射线加上总散射对分布函数（TSPDF）分析，通过研究样品的磺胺嘧啶，磺胺类抗生素药物，从冷冻研磨诱导的无定形状态重结晶。在不同条件下研磨的样品显示出具有显著不同的相组成。通过低温研磨稳定的1型多晶型物获得初始无定形状态。然后将其在低温下老化以引发受控的再结晶。我们表明，根据研磨和老化方案，我们看到无定形材料与亚稳2型多晶型物的混合物。还观察到少数形式1。我们描述的方法，使我们能够量化的相分数，尽管大多数样品缺乏结晶顺序。
One of the most challenging problems facing the pharmaceutical industry is to identify and quantify the phase fractions in mixed phase samples that contain crystalline, nanocrystalline, and amorphous components. Here we demonstrate an approach that accomplishes this using high energy X-rays coupled with total scattering pair distribution function (TSPDF) analysis by studying samples of sulfamer- azine, a sulfonamide antibiotic drug, recrystallizing from a cryomilled-induced amorphous state. Samples milled under different conditions were shown to have significantly different phase compositions. The initial amorphous state was obtained by cryomilling the stable Form 1 polymorph. This was then aged at low temperature to initiate controlled recrystallization. We show that depending on the milling and aging protocol we see a mixture of amorphous material with the metastable Form 2 polymorph. A minority of Form 1 is also observed. We describe the approach that allowed us to quantify the phase fractions despite the majority of the sample lacking crystalline order.