亚微米固定相毛细管电色谱法测定牛奶中磺胺类药物残留  

Determination of sulfonamides in milk with pressurized capillary electrochromatography based on sub-micron stationary phase

作　　者：申琳 柳青 陈巧梅[1] 薛芸[1] 王彦[1] 阎超[1] SHEN Lin;LIU Qing;CHEN Qiao-mei;XUE Yun;WANG Yan;YAN Chao(School of Pharmacy,Shanghai Jiao Tong University,Shanghai 20024)

机构地区：[1]上海交通大学药学院,上海200240

出　　处：《分析试验室》2018年第8期921-926,共6页Chinese Journal of Analysis Laboratory

基　　金：上海市科委科研计划项目(16142200300;17142201000);上海市引进技术的吸收与创新专项(XC-ZXSJ-02-2016-11);上海市标准化推进专项(17DZ2201500)资助

摘　　要：采用改良的St9ber法合成了780 nm和830 nm的亚微米色谱填料,制备了填充高度均匀的毛细管色谱填充柱,并与填充常规1.8μm和3μm色谱填料的毛细管柱对比,发现色谱固定相粒径越小,电渗流贡献率越大。结合亚微米填料和p CEC平台,建立了牛奶中5种磺胺类药物残留的固相萃取-p CEC分析方法,5 min内实现完全分离。结果显示5种磺胺类药物在0.1~10.0 mg/L浓度范围内线性良好(R2≥0.9990),检出限为0.02~0.04 mg/L,平均回收率为86.5%~98.8%(磺胺除外)。An improved St9 ber method was used to prepare the sub-micron particles of 780 nm and830 nm for uniformly packed columns. Compared with the regular chromatography medium of 1. 8μm and 3 μm,the percentage of EOF in whole velocity was larger with smaller particle size. The packed capillary column with 780 nm C18 bonded silica particles was applied in the determination of five sulfonamides in milk. The five sulfonamides were completely separated in 5 minutes. The results indicated that the linear rang was 0. 1 ~ 10. 0 mg/L（R2≥0. 9990）,the limit of detection was 0. 02-0. 04 mg/L, and the average recovery was 86. 5 % -98. 8 %（except for sulfonamide）.

关 键 词：亚微米色谱固定相 加压毛细管电色谱 电渗流 磺胺类药物 

分 类 号：TS207.5[轻工技术与工程—食品科学]