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采用UPLC-MS/MS建立了鸡蛋中16种磺胺类药物残留检测方法。样品经过磷酸盐缓冲液提取、正己烷分步去脂,氮吹、MCX柱净化后,经Acquity UPLC BEH(100 mm×2.1 mm,1.7μm)分离,以甲醇和0.1%加酸水溶液为流动相进行梯度洗脱,16种化合物能在11 min完全分离,方法的定量限均低于1.0μg/kg,在2.5~100μg/L范围内,16种磺胺类药物线性良好,相关系数均在0.99以上;通过2,10,40μg/kg加标回收实验表明,回收率为62.7%~96.1%,RSD为2.1%~15%。方法满足鸡蛋中磺胺类药物残留检测要求。
UPLC-MS / MS was used to establish a method for the determination of 16 sulfonamide residues in eggs. The sample was extracted with phosphate buffer, fractionated in n-hexane, slurried with nitrogen, purged with MCX column and separated by Acquity UPLC BEH (100 mm × 2.1 mm, 1.7 μm). The mobile phase consisted of methanol and 0.1% 16 compounds were completely separated at 11 min. The limits of quantification were less than 1.0μg / kg. The linear range of 16 sulfonamides was 2.5 ~ 100μg / L with the correlation coefficients above 0.99 The recoveries of 2, 10 and 40 μg / kg spiked recoveries ranged from 62.7% to 96.1% with RSD ranging from 2.1% to 15%. Methods to meet the detection requirements of sulfa residues in eggs.