Al-Kindy Salma M Z, Al-Wishahi Aisha, Suliman Fakhr Eldin O
Department of Chemistry, College of Science, Sultan Qaboos University, P. Box 36, Al-Khod 123, Oman.
Talanta. 2004 Dec 15;64(5):1343-50. doi: 10.1016/j.talanta.2004.04.014.
A simple, selective and sensitive luminescence method for the assay of piroxicam (PX) in pharmaceutical formulation is developed. The method is based on the luminescence sensitization of europium (Eu(3+)) by complexation with PX. The signal for PX-EU is monitored at lambda(ex)=358nm and lambda(em)=615nm. Optimum conditions for the formation of the complex in methanol were 0.01M TRIS buffer and 0.2mM of Eu(3+) which allows the determination of 100-2000ppb of pX in batch method and 100-1000ppb with limit of detection (LOD) = 23.0ppb using sequential injection analysis (SIA). The relative standard deviations of the method range between 2 and 3% indicating excellent reproducibility of the method. The proposed method was successfully applied for he assay of PX in pharmaceutical formulations (Feldene capsules and tablets). Average recoveries of 101.0+/-0.3 and 98.8+/-2.7% were obtained for capsules in methanol using batch and sequential injection (SI) methods, respectively.
开发了一种用于测定药物制剂中吡罗昔康(PX)的简单、选择性和灵敏的发光方法。该方法基于吡罗昔康(PX)与铕(Eu(3+))络合对铕(Eu(3+))的发光增敏作用。在激发波长(λ(ex))=358nm和发射波长(λ(em))=615nm处监测PX-Eu的信号。在甲醇中形成络合物的最佳条件是0.01M三羟甲基氨基甲烷(TRIS)缓冲液和0.2mM的Eu(3+),这使得在分批法中可测定100-2000ppb的PX,使用顺序注射分析(SIA)时可测定100-1000ppb,检测限(LOD)=23.0ppb。该方法的相对标准偏差在2%至3%之间,表明该方法具有出色的重现性。所提出的方法成功应用于药物制剂( Feldene胶囊和片剂)中PX的测定。使用分批法和顺序注射(SI)法在甲醇中测定胶囊时,平均回收率分别为101.0±0.3%和98.8±2.7%。