Mazurek-Wadołkowska Edyta, Winnicka Katarzyna, Czajkowska-Kośnik Anna, Czyzewska Urszula, Miltyk Wojciech
Department of Pharmaceutical Technology, Medical University of Białystok, Mickiewicza 2c, 15-222 Białystok, Poland.
Acta Pol Pharm. 2013 Sep-Oct;70(5):787-93.
Differential scanning calorimetry (DSC) is an analytical procedure used to determine the differences in the heat flow generated or absorbed by the sample. This method allows to assess purity and polymorphic form of drug compounds, to detect interactions between ingredients of solid dosage forms and to analyze stability of solid formulations. The aim of this study was the assessment of compatibility between acetaminophen (API) and different types of excipients often used in tablets compression: polyvinylpyrrolidone, crospovidone, pregelatinized starch, microcrystalline cellulose and magnesium stearate by differential scanning calorimetry. The study contains results of thermal analysis of excipients and individually performed mixtures of these substances with acetaminophen before and after compression and after 6 months storage of tablets at different temperature and relative humidity conditions (25 +/- 2 degrees C /40 +/- 5% RH, 25 +/- 2 degrees C /60 +/- 5% RH, 40 +/- 2 degrees C /75 +/- 5% RH) for a period of 6 months. To detect possible changes of API chemical structure, gas chromatography-mass spectrometry (GC-MS) was also applied. GC-MS with electron impact ionization (EI) was employed to determine the fragmentation pattern of API. It was shown that the developed formulations showed excellent compatibility among all excipients used except Kollidon CL. The interaction with Kollidon CL is probably a result of a physical reaction as confirmed by GC-MS analyses. Obtained results revealed that DSC can be successfully applied to evaluate possible incompatibilities between acetaminophen and Kollidon.
差示扫描量热法（DSC）是一种用于确定样品产生或吸收的热流差异的分析方法。该方法可用于评估药物化合物的纯度和多晶型形式，检测固体剂型成分之间的相互作用，并分析固体制剂的稳定性。本研究的目的是通过差示扫描量热法评估对乙酰氨基酚（原料药）与片剂压片中常用的不同类型辅料（聚乙烯吡咯烷酮、交联聚维酮、预胶化淀粉、微晶纤维素和硬脂酸镁）之间的相容性。该研究包含了对辅料以及这些物质与对乙酰氨基酚在压片前后以及在不同温度和相对湿度条件（25±2℃/40±5%RH、25±2℃/60±5%RH、40±2℃/75±5%RH）下储存6个月后的单独混合物进行热分析的结果。为了检测原料药化学结构的可能变化，还应用了气相色谱 - 质谱联用（GC - MS）。采用带有电子轰击电离（EI）的GC - MS来确定原料药的碎片模式。结果表明，所开发的制剂在除聚乙烯吡咯烷酮CL之外使用的所有辅料之间显示出优异的相容性。GC - MS分析证实，与聚乙烯吡咯烷酮CL的相互作用可能是物理反应的结果。所得结果表明，DSC可成功应用于评估对乙酰氨基酚与聚乙烯吡咯烷酮之间可能的不相容性。
