Mostafa Islam M, Omar Mahmoud A, Nagy Dalia M, Derayea Sayed M
Analytical Chemistry Department, Faculty of Pharmacy, Minia University Minia Egypt
RSC Adv. 2018 Jun 15;8(39):22154-22160. doi: 10.1039/c8ra03614d. eCollection 2018 Jun 13.
Our article presents the development and validation of two simple, very sensitive, and low-cost spectroscopic methods for the assay of milnacipran hydrochloride in bulk form, pharmaceutical tablets and spiked human urine and plasma. Spectroscopic methods (spectrophotometric and spectrofluorimetric techniques) were dependent on the chromogenic and fluorogenic properties of the 4-chloro-7 nitrobenzofurazan (NBD-Cl) reagent. The reaction product, resulting from the interaction between NBD-Cl and milnacipran in the presence of borate buffer pH 8.5, was measured spectrophotometrically at 465 nm and spectrofluorimetrically at 510 nm after excitation at 465 nm. The absorbance-concentration plot was rectilinear over the range of 1.5-12 μg mL with a limit of quantitation 1.09 μg mL, while the fluorescence-concentration plot was rectilinear over the range of 0.03-0.5 μg mL with a limit of quantitation 0.02 μg mL. Influential parameters affecting the development and stability of the reaction product were studied and optimized. Assurance of the cited drug in its tablets by our proposed methods was successfully completed without obstruction from the presence of the basic excipients with average percentage recoveries of 99.27 ± 1.18 and 99.44 ± 0.69 for the spectrophotometric and spectrofluorimetric methods, respectively. The spectrofluorimetric method was additionally adopted as a preliminary study for the assay of the cited drug in spiked human urine and plasma with average percentage recoveries of 101.52 ± 1.01 and 100.38 ± 1.57 for spiked urine and plasma, respectively.
我们的文章介绍了两种简单、灵敏度极高且成本低廉的光谱法的开发与验证，这两种方法用于测定散装形式、药物片剂以及加标人尿和血浆中的盐酸米那普明。光谱法（分光光度法和荧光分光光度法技术）依赖于4-氯-7-硝基苯并呋喃（NBD-Cl）试剂的显色和荧光特性。在pH 8.5的硼酸盐缓冲液存在下，NBD-Cl与米那普明相互作用产生的反应产物，在465 nm处进行分光光度测定，在465 nm激发后于510 nm处进行荧光分光光度测定。吸光度-浓度曲线在1.5 - 12 μg/mL范围内呈线性，定量限为1.09 μg/mL，而荧光-浓度曲线在0.03 - 0.5 μg/mL范围内呈线性，定量限为0.02 μg/mL。研究并优化了影响反应产物生成和稳定性的相关参数。通过我们提出的方法成功完成了片剂中所述药物的测定，不受碱性辅料存在的干扰，分光光度法和荧光分光光度法的平均回收率分别为99.27 ± 1.18和99.44 ± 0.69。荧光分光光度法还被用作加标人尿和血浆中所述药物测定的初步研究，加标尿和血浆的平均回收率分别为101.52 ± 1.01和100.38 ± 1.57。
