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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 13 sulfonamides residues in milk by solid phase extraction and high performance liquid chromatography was established. After the sample was extracted by acetonitrile by swirling ultrasonic waves, the sample was purified by self-made alkaline alumina solid phase extraction cartridge (SPE). The eluate was concentrated under reduced pressure to near dryness and then dissolved in a mobile phase and fixed. After passing through a PTFE filter, Scientific ODS hypersil column with gradient elution with acetonitrile-20 mmol / L H3PO4 as the mobile phase at a detection wavelength of 270 nm. Thirteen sulfonamides showed a good linearity in the range of 50-5000 μg / L, the correlation coefficient was ≥0.999, the detection limit was 2.0-4.2 μg / L and the limit of quantification was 8.9-14.2 μg / L. The spiked recoveries at 20, 50 and 100 μg / L ranged from 79.0% to 118.2% with relative standard deviations between 2.7% and 6.9%. The method can accurately and quantitatively analyze the 13 sulfonamides residues in milk.