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

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）.