固相萃取-高效液相色谱法同时测定牛奶中13种磺胺残留

Solid-phase extraction combined with high-performance liquid chromatographic method for simultaneous determination of thirteen sulfonamides in milk

建立了固相萃取-高效液相色谱同时测定牛奶中13种磺胺类药物残留的方法。样品经乙腈溶液漩涡超声提取后,采用自制碱性氧化铝固相萃取小柱（SPE）净化,洗脱液减压浓缩至近干后用流动相溶解并定容,过PTFE滤膜后在Thermo Fisher Scientific ODS hypersil色谱柱上,以乙腈-20 mmol/L H3PO4溶液为流动相进行梯度洗脱,检测波长为270 nm。13种磺胺在50-5000μg/L范围内具有良好的线性,相关系数≥0.999,检出限为2.0-4.2μg/L,定量限为8.9-14.2μg/L。在20,50,100μg/L添加水平的加标回收率为79.0%-118.2%,相对标准偏差在2.7%-6.9%之间。方法能对牛奶中13种磺胺类药物残留实现准确定量分析。

A method for simultaneous determination of thirteen sulfonamides in milk by homemade solid-phase extraction （SPE） combined with high-performance liquid chromatography （HPLC） has been established. The samples were extracted by acetonitrile solution, the solution were enriched and cleaned up by homemade alumina-B solid-phase extraction cartridges, and then were analyzed by HPLC at the wavelength of 270 nm. The chromatographic separation was performed on a Thermo Fisher Scientific ODS hypersil column mmoL/L phosphoric acid solution-acetonitrile as the mobile phase. The recoveries of 3 dyes ranged by using 20 from 79.0% to 118.2%, and the relative standard deviations （RSDs） were 2.7% - 6.9% （n = 5 ）. The calibration curve was linear in the range of 50 - 5000 μg,/L with the correlation coefficients of more than 0. 999. The limits of detection were from 2.0 to 4. 2 μg/Land the limits of quantitation were from 8.9 to 14. 2 μg/L for thirteen sulfonamides. The method showed good repeatability, accuracy and stability, and it could be applied to the accurate quantification of thirteen sulfonamides in milk.