Shah Jasmin, Jan Muhammad Rasul, Khan Muhammad Naeem, Shah Sultan
Institute of Chemical Sciences, University of Peshawar, Peshawar, Pakistan.
Pak J Pharm Sci. 2013 Sep;26(5):921-8.
A simple, sensitive, selective and cost effective spectrofluorimetric method has been established for the quantification of sulpiride after their complete alkaline hydrolysis. The method is based on the condensation of the primary amino group of alkaline hydrolytic product of sulpiride with acetyl acetone and formaldehyde in acidic medium (0.25 M HCl) to form a fluorescent product. The reaction product formed shows maximum fluorescence intensity at 483 nm after excitation at 431 nm. The different reaction conditions influencing the condensation reaction were carefully optimized and a linear range of 0.1-3.5 µg mL-1 with good correlation coefficient between flourescent intensity and concentration of sulpiride was found at optimum parameters. The LOD and LOQ were found to be 11 and 39 ng mL-1 respectively. The proposed method was successfully used for the quantification of sulpiride in bulk powder and commercial formulations. The effect of common pharmaceutical excipients and co-administered drug was also studied and no interferences were observed. The validity of the method was tested by analyzing sulpiride in bulk powder, and pharmaceutical formulations through recovery studies. Recoveries (%) were obtained from 98.62 to 100.24% for bulk powder, and 97.09 to 100.57 % for commercial formulations. The results were validated statistically with those obtained by reference literature high performance liquid chromatographic method.
已建立一种简单、灵敏、选择性好且成本效益高的荧光分光光度法，用于在舒必利完全碱性水解后对其进行定量分析。该方法基于舒必利碱性水解产物的伯氨基在酸性介质（0.25 M HCl）中与乙酰丙酮和甲醛缩合形成荧光产物。形成的反应产物在431 nm激发后，于483 nm处显示最大荧光强度。仔细优化了影响缩合反应的不同反应条件，在最佳参数下发现荧光强度与舒必利浓度之间的线性范围为0.1 - 3.5 µg mL-1，具有良好的相关系数。检测限和定量限分别为11和39 ng mL-1。所提出的方法成功用于散装粉末和市售制剂中舒必利的定量分析。还研究了常见药用辅料和共同给药药物的影响，未观察到干扰。通过对散装粉末和药物制剂中的舒必利进行回收率研究来测试该方法的有效性。散装粉末的回收率（%）为98.62至100.24%，市售制剂的回收率为97.09至100.57%。将结果与参考文献高效液相色谱法获得的结果进行统计学验证。
