Omar Mahmoud A, Abdelmageed Osama H, Attia Tamer Z
Analytical Chemistry Department, Faculty of Pharmacy, Minia University, Minia, Egypt.
Talanta. 2009 Feb 15;77(4):1394-404. doi: 10.1016/j.talanta.2008.09.040. Epub 2008 Oct 4.
An accurate, reliable, specific and sensitive kinetic spectrofluorimetric method was developed for the determination of seven cephalosporin antibiotics namely cefotaxime sodium, cephapirin sodium, cephradine dihydrate, cephalexin monohydrate, cefazoline sodium, ceftriaxone sodium and cefuroxime sodium. The method is based on their degradation under an alkaline condition producing fluorescent products. The factors affecting the degradation and the determination were studied and optimized. The reaction is followed spectrofluorimetrically by measuring the rate of change of fluorescence intensity at specified emission wavelength. The initial rate and fixed time methods were used for the construction of calibration graphs to determine the concentration of the studied drugs. The calibration graphs are linear in the concentration ranges 0.2-1.2 microg mL(-1) and 0.2-2.2 microg mL(-1) using the initial rate and fixed time methods, respectively. The results were statistically validated and checked through recovery studies. The method has been successfully applied for the determination of the studied cephalosporins in commercial dosage forms. The high sensitivity of the proposed method allows the determination of investigated cephalosporins in human plasma. The statistical comparisons of the results with the reference methods show an excellent agreement and indicate no significant difference in accuracy and precision.
建立了一种准确、可靠、特异且灵敏的动力学荧光光谱法，用于测定7种头孢菌素抗生素，即头孢噻肟钠、头孢匹林钠、头孢拉定二水合物、头孢氨苄一水合物、头孢唑林钠、头孢曲松钠和头孢呋辛钠。该方法基于它们在碱性条件下降解产生荧光产物。研究并优化了影响降解和测定的因素。通过在特定发射波长下测量荧光强度的变化速率，用荧光光谱法跟踪反应。采用初始速率法和固定时间法绘制校准曲线，以测定所研究药物的浓度。使用初始速率法和固定时间法时，校准曲线分别在0.2 - 1.2 μg mL⁻¹和0.2 - 2.2 μg mL⁻¹的浓度范围内呈线性。通过回收率研究对结果进行了统计学验证和检验。该方法已成功应用于商业剂型中所研究头孢菌素的测定。所提出方法的高灵敏度使得能够测定人血浆中的被研究头孢菌素。结果与参考方法的统计学比较显示出极好的一致性，表明在准确度和精密度方面无显著差异。
