SPE及纳米金涂层毛细管电泳检测血浆中土霉素与多西环素

Determination of Oxytertracycline and Doxycycline in Plasma by SPE and Au NPs Coated Capillary Electrophoresis

建立了混合型固相萃取及季铵化纤维素负载的纳米金涂层毛细管电泳法快速检测血浆中土霉素和多西环素的方法。采用季铵化纤维素负载的纳米金复合材料（QC-Au NPs）对毛细管内壁进行动态涂层,以抑制管壁对分析物的吸附,并对缓冲液p H值进行优化。结果表明,该涂层能改善峰形和分离度,提高分离效率,其中土霉素的柱效提高了17.9倍。在涂层毛细管中,土霉素和多西环素的吸附被抑制,并在4 min内出峰。在10~200μg/m L范围内,土霉素和多西环素的峰面积与浓度的线性关系良好,相关系数（r）分别为0.997 6和0.995 2。血浆中土霉素和多西环素的加标回收率为88%~107%,相对标准偏差（RSD）为1.4%~7.7%。该方法快速、简便,准确度和精密度高,适用于血浆中土霉素和多西环素的快速检测。

A method for the rapid determination of oxytertracycline and doxycycline in plasma was established by mix mode solid phase extraction（ SPE） and quaternized cellulose supported Au nanoparticles（ QC- Au NPs） coated capillary electrophoresis. The QC- Au NPs were used to coat the capillary inner surface and inhibit the adsorption of analyte. The p H value of running buffer was also optimized. The result showed that the peak shape and resolution were improved,and the separation efficiency was also increased. The number of theoretical plates of oxytertracycline increased by 17. 9times as compared with that of inner bare capillary. The adsorption of oxytertracycline and doxycycline was inhibited in the capillary coated with QC- Au NPs,and their analysis could be completed in4 min. Good linearities were obtained for oxytertracycline and doxycycline in the range of 10- 200μg /m L,with correlation coefficients of 0. 997 6 and 0. 995 2,respectively. The recoveries of the analytes in plasma at three spiked levels ranged from 88% to 107%,and the relative standard deviations（ RSDs） ranged from 1. 4%- 7. 7%. This method is rapid,simple and accurate,and is feasible for the determination of oxytertracycline and doxycycline in plasma samples.