Institute of Chemical Sciences, University of Peshawar, Peshawar, Pakistan; Department of Chemistry, Kyungpook National University, Daegu, 702-701, South Korea.
Luminescence. 2013 Nov-Dec;28(6):915-21. doi: 10.1002/bio.2458. Epub 2012 Dec 6.
A highly sensitive and simple method for identifying sulpiride in pharmaceutical formulations and biological fluids is presented. The method is based on increased chemiluminescence (CL) intensity of a luminol-H2O2 system in response to the addition of Cr (III) under alkaline conditions. The CL intensity of the luminol-H2O2-Cr (III) system was greatly enhanced by the addition of sulpiride and the CL intensity was proportional to the concentration of sulpiride in a sample solution. Various parameters affecting the CL intensity were systematically investigated and optimized for determination of the sulpiride in a sample. Under the optimum conditions, the CL intensity was proportional to the concentration of sulpiride in the range of 0.068-4.0 µg/mL, with a good correlation coefficient of 0.997. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 8.50 × 10(-6) µg/mL and 2.83 × 10(-5) µg/mL, respectively. The method presented here produced good reproducibility with a relative standard deviation (RSD) of 2.70% (n = 7). The effects of common excipients and metal ions were studied for their interference effect. The method was validated statistically through recovery studies and successfully applied for the determination of sulpiride in pure form, pharmaceutical preparations and spiked human plasma samples. The percentage recoveries were found to range from 99.10 to 100.05% for pure form, 98.12 to 100.18% for pharmaceutical preparations and 97.9 to 101.4% for spiked human plasma.
一种用于鉴定药物制剂和生物体液中舒必利的高灵敏度且简单的方法被提出。该方法基于在碱性条件下加入三价铬（III）时，鲁米诺-H2O2 体系的化学发光（CL）强度增加。鲁米诺-H2O2-Cr（III）体系的 CL 强度在加入舒必利后大大增强，并且 CL 强度与样品溶液中舒必利的浓度成正比。系统地研究了影响 CL 强度的各种参数，并对样品中的舒必利进行了优化。在最佳条件下，CL 强度与舒必利的浓度在 0.068-4.0 µg/mL 范围内成正比，具有良好的相关系数为 0.997。检测限（LOD）和定量限（LOQ）分别为 8.50 × 10(-6) µg/mL 和 2.83 × 10(-5) µg/mL。所提出的方法具有良好的重现性，相对标准偏差（RSD）为 2.70%（n = 7）。研究了常见赋形剂和金属离子对其干扰效应的影响。该方法通过回收率研究进行了统计学验证，并成功应用于纯形式、药物制剂和加标人血浆样品中舒必利的测定。对于纯形式，回收率范围为 99.10%至 100.05%；对于药物制剂，回收率范围为 98.12%至 100.18%；对于加标人血浆，回收率范围为 97.9%至 101.4%。
