Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Al-Azhar University, Assiut Branch, Assiut 71524, Egypt.
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Al-Azhar University, Assiut Branch, Assiut 71524, Egypt.
Spectrochim Acta A Mol Biomol Spectrosc. 2021 Mar 5;248:119165. doi: 10.1016/j.saa.2020.119165. Epub 2020 Nov 12.
Baclofen belongs to skeletal muscle relaxant and is used for the treatment of muscle spasticity that originated from multiple sclerosis or a spinal cord injury and other cases as hiccups. In the current analytical study, a new, convenient and selective fluorimetric method for baclofen analysis has been developed and validated. The analytical methodology depends on Hantzsch reaction that leads to formation of dihydropyridine fluorescent derivative. The primary amino moiety in baclofen condensed with two equivalents of acetylacetone in the presence of formaldehyde and acetate buffer solutions. Spectrofluorimetric monitoring of the product was accomplished at emission wavelength of 477.3 nm after excitation at 419.9 nm. The method exhibited linearity when baclofen concentration plotted against the fourescence response in the range of 0.3-6.0 µg/mL. Adjustment of the reaction variables and studying validation parameters according to directives of ICH were performed perfectly. Ultimately, the proposed approach was applied successfully for baclofen analysis in raw material, dosage form and spiked urine and it was also extended to test content uniformity.
巴氯芬属于骨骼肌松弛剂,用于治疗多发性硬化症或脊髓损伤等引起的肌肉痉挛和其他病例的打嗝。在当前的分析研究中,开发并验证了一种新的、方便的和选择性的荧光光度法来分析巴氯芬。该分析方法依赖于 Hantzsch 反应,该反应导致二氢吡啶荧光衍生物的形成。在存在甲醛和醋酸盐缓冲溶液的情况下,巴氯芬的伯氨基与两倍当量的乙酰丙酮缩合。产物的光谱荧光监测在激发波长为 419.9nm 后,在 477.3nm 的发射波长处完成。当巴氯芬浓度与荧光响应在 0.3-6.0μg/mL 的范围内作图时,该方法表现出线性关系。根据 ICH 的指令,完美地调整了反应变量并研究了验证参数。最终,该方法成功地应用于原料药、制剂和加标尿液中的巴氯芬分析,并扩展到测试含量均匀度。