Ghoneim M M, Beltagi A M
Department of Chemistry, Faculty of Science, Tanta University, Tanta, Egypt.
Talanta. 2003 Jul 27;60(5):911-21. doi: 10.1016/S0039-9140(03)00151-6.
Celecoxib is a cyclooxygenase inhibitor, that has been recently and intensively prescribed as an anti-inflammatory drug in rheumatic osteoarthritis. A robust, highly reliable and reproducible square-wave (SW) adsorptive cathodic stripping voltammetric procedure was developed for the determination of celecoxib in pharmaceutical formulation and human serum. The analytical procedure was based on the reduction of the CN of the pyrazole ring of the drug molecule at the mercury electrode surface in Britton-Robinson buffer of pH 7.0. The SW adsorptive cathodic stripping voltammogram of celecoxib showed a single well-defined peak at -1.54 V (vs. Ag/AgCl/KCl(s)) using an accumulation potential of -0.70 V, frequency of 120 Hz, scan increment of 10 mV and pulse amplitude of 25 mV. Repeatability was examined for 1 x 10(-8) M CXB drug solution after 30 s pre-concentration and a mean recovery of 99.4+/-0.4% (n=5) was achieved. For 90 s preconcentration, a linear concentration range of 1 x 10(-9)-2 x 10(-8) M CXB and a detection limit of 1.86 x 10(-10) M were achieved. The proposed procedure was successfully applied for the determination of the drug in capsules and human serum with mean recoveries of 101.5+/-0.6 and 98.8+/-1.1%, respectively. A detection and quantitation limits of 1.0 x 10(-9) M (0.4 ng ml(-1)) and 4.7 x 10(-9) M (1.3 ng ml(-1)) were achieved for the determination of the drug in human serum. Moreover, the procedure was useful for study of the pharmacokinetic profile of celecoxib in a healthy volunteer after administration of a single oral dose (celebrex, 200 mg).
塞来昔布是一种环氧化酶抑制剂，最近在风湿性骨关节炎中作为抗炎药物被大量且频繁地使用。本文建立了一种稳健、高度可靠且可重复的方波吸附阴极溶出伏安法，用于测定药物制剂和人血清中的塞来昔布。该分析方法基于在pH 7.0的Britton-Robinson缓冲液中，药物分子吡唑环上的氰基在汞电极表面的还原反应。使用-0.70 V的富集电位、120 Hz的频率、10 mV的扫描增量和25 mV的脉冲幅度时，塞来昔布的方波吸附阴极溶出伏安图在-1.54 V（相对于Ag/AgCl/KCl(s)）处显示出一个清晰明确的单峰。对1×10⁻⁸ M的塞来昔布药物溶液进行30 s预富集后，考察了方法的重复性，平均回收率为99.4±0.4%（n = 5）。预富集90 s时，塞来昔布的线性浓度范围为1×10⁻⁹ - 2×10⁻⁸ M，检测限为1.86×10⁻¹⁰ M。所提出的方法成功应用于胶囊和人血清中药物的测定，平均回收率分别为101.5±0.6%和98.8±1.1%。测定人血清中的药物时，检测限和定量限分别为1.0×10⁻⁹ M（0.4 ng ml⁻¹）和4.7×10⁻⁹ M（1.3 ng ml⁻¹）。此外，该方法有助于研究健康志愿者单次口服剂量（西乐葆，200 mg）后塞来昔布的药代动力学特征。
