Maślanka Anna, Krzek Jan, Patrzałek Aleksander
Department of Inorganic and Analytical Chemistry, Jagiellonian University, Collegium Medicum, 9 Medyczna St., 30-688 Kraków, Poland.
Acta Pol Pharm. 2009 Sep-Oct;66(5):461-70.
New chromatographic-densitometric assay was developed for identification and determination of risperidone in pharmaceutical formulations. Thin-layer chromatographic plates (TLC-F254) as a stationary phase and n-butanol-acetic acid-water (12:3:5 v/v/v) as a mobile phase were used for separation. Densitometric measurements were done for all constituents at lambda = 280 nm. A decrease in stability of risperidone was observed in acidic, basic and antioxidant solutions. Degradation of active pharmaceutical ingredient was consistent with first-order kinetics and unrelated to the solution. This assay is specific for risperidone. No interference of tablet origin adjuvants and degradation products were observed. Moreover, high sensitivity, limit of detection (0.22 microg/spot), limit of quantitation (0.67 microg/spot), recovery (98.2-100.82%), broad linear range (0.09 microg/spot to 1.40 microg/spot) and accuracy (1.87% RSD) are characteristic traits of the chromatographic-densitometric assay.
开发了一种新的色谱 - 密度测定法，用于鉴定和测定药物制剂中的利培酮。采用薄层色谱板（TLC - F254）作为固定相，正丁醇 - 乙酸 - 水（12:3:5 v/v/v）作为流动相进行分离。在λ = 280 nm处对所有成分进行密度测定。在酸性、碱性和抗氧化剂溶液中观察到利培酮的稳定性降低。活性药物成分的降解符合一级动力学，且与溶液无关。该测定法对利培酮具有特异性。未观察到片剂辅料和降解产物的干扰。此外，高灵敏度、检测限（0.22μg/斑点）、定量限（0.67μg/斑点）、回收率（98.2 - 100.82%）、宽线性范围（0.09μg/斑点至1.40μg/斑点）和准确度（1.87%相对标准偏差）是色谱 - 密度测定法的特征。
