Deng Biyang, Kang Yanhui, Li Xianfeng, Xu Qiumei
College of Chemistry and Chemical Engineering, Guangxi Normal University, Guilin 541004, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Nov 1;859(1):125-30. doi: 10.1016/j.jchromb.2007.09.014. Epub 2007 Sep 18.
A novel determination method for josamycin (JOS) based on capillary electrophoresis-electrochemiluminescence detection has been described. In this study, platinum disk electrode (300 microm in diameter) was used as a working electrode and the conditions affecting separation and detection were investigated in detail. Under optimal condition: 40 cm separation capillary (75 microm i.d.); 1.25 V applied potential on the Pt disc of the ECL detector cell; 5 mM Ru(bpy)3(2+) and 50mM phosphate buffer (pH 7.5) in the detection cell; 12 kV separation voltage; 8s injection time; 10 kV injection voltage and 15 mM running buffer (pH 7.5), calibration curve was linear over the range from 10 ng/mL to 5.0 microg/mL with a detection limit of 3.1 ng/mL at a signal-to-noise ratio of 3. The method can be successfully applied for the determination of josamycin in rat plasma in 6 min and the extraction recoveries with spiked plasma samples were over 92%.
本文描述了一种基于毛细管电泳-电化学发光检测的新型交沙霉素(JOS)测定方法。本研究中,使用直径为300微米的铂盘电极作为工作电极,并详细研究了影响分离和检测的条件。在最佳条件下:40厘米分离毛细管(内径75微米);在ECL检测池的铂盘上施加1.25伏的电位;检测池中含有5毫摩尔的Ru(bpy)3(2+)和50毫摩尔的磷酸盐缓冲液(pH 7.5);12千伏分离电压;8秒进样时间;10千伏进样电压和15毫摩尔运行缓冲液(pH 7.5),校准曲线在10纳克/毫升至5.0微克/毫升范围内呈线性,在信噪比为3时检测限为3.1纳克/毫升。该方法可在6分钟内成功用于测定大鼠血浆中的交沙霉素,加标血浆样品的提取回收率超过92%。