School of Chemistry and Chemical Engineering, Southwest University, Chongqing, China.
Luminescence. 2013 Mar-Apr;28(2):211-6. doi: 10.1002/bio.2365. Epub 2012 Jun 5.
A novel, sensitive and rapid CL method coupled with high-performance liquid chromatography separation for the determination of carbamazepine is described. The method was based on the fact that carbamazepine could significantly enhance the chemiluminescence of the reaction of cerium sulfate and tris(2,2-bipyridyl) ruthenium(II) in the presence of acid. The chromatographic separation was performed on a Kromasil® (Sigma-Aldrich) TM RP-C18 column (id: 150 mm × 4.6 mm, particle size: 5 µm, pore size: 100 Å) with a mobile phase consisting of methanol-water-glacial acetic acid (70:29:1, v/v/v) at a flowrate of 1.0 mL/min, the total analysis time was within 650 s. Under optimal conditions, CL intensity was linear for carbamazepine in the range 2.0 × 10(-8) ~ 4.0 × 10(-5) g/mL, with a detection limit of 6.0 × 10(-9) g/mL (S/N = 3) and the relative standard detection was 2.5% for 2.0 × 10(-6) g/mL (n = 11). This method was successfully applied to the analysis of carbamazepine in human urine and serum samples. The possible mechanism of the CL reaction is also discussed briefly.
一种新型、灵敏、快速的化学发光（CL）方法结合高效液相色谱分离用于测定卡马西平。该方法基于以下事实：在酸性条件下，卡马西平可显著增强硫酸铈和三（2,2-联吡啶）钌（II）反应的化学发光。色谱分离在 Kromasil®（Sigma-Aldrich）TM RP-C18 柱（id：150mm×4.6mm，粒径：5μm，孔径：100Å）上进行，流动相由甲醇-水-冰醋酸（70:29:1，v/v/v）组成，流速为 1.0mL/min，总分析时间在 650s 内。在最佳条件下，CL 强度在 2.0×10(-8)~4.0×10(-5)g/mL 范围内与卡马西平呈线性关系，检测限为 6.0×10(-9)g/mL（S/N=3），相对标准检测为 2.5%（n=11），浓度为 2.0×10(-6)g/mL。该方法成功应用于人尿和血清样品中卡马西平的分析。还简要讨论了 CL 反应的可能机制。
