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基于稀土Eu(Ⅲ)掺杂的类普鲁士蓝膜修饰的铂电极为工作电极,建立了测定羟考酮的毛细管电泳-电致化学发光分析方法。考察了检测电位、运行缓冲溶液的酸度及浓度、分离电压、进样条件等对电泳分离效果及检测灵敏度的影响。在最佳的实验条件下,羟考酮可在4 min内得到分离,其ECL强度值与羟考酮的质量浓度在7.0×10-2～7.0μg/mL和7.0～70.0μg/mL范围内呈良好的线性关系,检出限为4.2×10-2μg/mL(3σ),峰高和迁移时间的相对偏差分别为3.6%和0.48%(n=6)。方法用于兔血浆中羟考酮含量的检测,加标回收率在99.7%～101.0%之间。
A capillary electrophoresis-electrochemiluminescence (PLG) method for the determination of oxycodone was established based on a platinum-like electrode modified with Eu (Ⅲ) -doped Prussian blue film as the working electrode. The influence of the detection potential, the acidity and concentration of the running buffer solution, the separation voltage and the injection conditions on the electrophoretic separation and detection sensitivity were investigated. Under the optimal experimental conditions, oxycodone could be separated within 4 min, and the ECL intensity value and the mass concentration of oxycodone were in the range of 7.0 × 10-2 ~ 7.0μg / mL and 7.0 ~ 70.0μg / mL The detection limit was 4.2 × 10-2 μg / mL (3σ). The relative deviations of peak height and migration time were 3.6% and 0.48%, respectively (n = 6). The method was applied to the determination of oxycodone in rabbit plasma with the recoveries of 99.7% -101.0%.