Shaalan Rasha Abdel-Aziz
Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Alexandria University, Elmessalah 21521, Alexandria, Egypt.
Int J Biomed Sci. 2010 Sep;6(3):260-7.
Three new, simple, sensitive and selective spectrofluorimetric and spectrophotometric methods were developed for the determination of the γ-amino-n-butyric acid derivative, pregabalin. Pregabalin as a primary amine reacts with fluorescamine to yield a fluorescent product (Method I), with 2,4-dinitrofluorobenzene (Method II) and 2,3,5,6-tetrachloro-1,4-benzoquinone (Method III) in aqueous alkaline buffered media to form colored products which could be measured spectrophotometrically. The optimum conditions for each reaction were ascertained and the methods were applied for the determination of pregabalin over the concentration range of 20-280 ng mL(-1) and 1-7 μg mL(-1) for spectrofluorimetry and spectrophotometry, respectively with good correlation (≥0.999). The limits of assays detection ranged from 9.6 × 10(-4) μg mL(-1) to 0.42 μg mL(-1) for spectrofluorimetry and spectrophotometry, respectively. The suggested methods were applied to the determination of the drug in capsules. No interference could be observed from the additives listed to be in capsules. Furthermore, the spectrofluorimetric method was extended to the in-vitro determination of pregabalin in spiked urine, interference from endogenous amino acids could be eliminated through selective complexation with copper acetate; the percentage recovery was found to be 98% ± 1.42 (n=6). Co- administered drugs such as chlordiazepoxide, clonazepam, diazepam, nitrazepam and lamotrigine did not interfere with the assay. The methods were validated with respect to linearity, accuracy, precision and robustness. The results obtained were determined to be in good agreement with those obtained using a previously reported method.
开发了三种新的、简单、灵敏且具有选择性的荧光分光光度法和分光光度法，用于测定γ-氨基丁酸衍生物普瑞巴林。普瑞巴林作为伯胺，在碱性缓冲水溶液介质中与荧光胺反应生成荧光产物（方法I），与2,4-二硝基氟苯（方法II）和2,3,5,6-四氯-1,4-苯醌（方法III）反应形成可通过分光光度法测定的有色产物。确定了每个反应的最佳条件，这些方法分别用于荧光分光光度法和分光光度法测定普瑞巴林，浓度范围分别为20 - 280 ng mL(-1)和1 - 7 μg mL(-1)，具有良好的相关性（≥0.999）。荧光分光光度法和分光光度法的检测限分别为9.6 × 10(-4) μg mL(-1)至0.42 μg mL(-1)。所建议的方法用于测定胶囊中的药物。未观察到胶囊中列出的添加剂产生干扰。此外，荧光分光光度法扩展到加标尿液中普瑞巴林的体外测定，通过与醋酸铜选择性络合可消除内源性氨基酸的干扰；回收率为98% ± 1.42（n = 6）。同时服用的药物如氯氮卓（利眠宁）、氯硝西泮、地西泮、硝西泮和拉莫三嗪不干扰测定。这些方法在线性、准确度、精密度和稳健性方面进行了验证。所得结果与使用先前报道的方法获得的结果高度一致。
