该研究建立了动物源性食品中19种磺胺类药物残留的确证检测方法，利用盐包和流穿式净化柱对动物源性食品进行双重净化，并采用超高效液相色谱-串联质谱（UPLC-MS/MS）进行检测分析。样品经80%乙腈（0.2%甲酸）提取、盐包及Speedy Prep®-Sulfa流穿式净化柱净化，使用ACQUITY UPLC BEH C18色谱柱分离，以0.2%甲酸水和甲醇作为流动相进行梯度洗脱，质谱采用电喷雾正离子模式和多反应监测模式采集信号，外标法定量分析。结果表明，该方法中流穿式净化柱可在30 s内完成净化，整个前处理过程缩短至10 min以内。19种磺胺类药物在其线性范围内相关系数r≥0.999 1，检出限为1.00~2.00 μg/kg，定量限为2.50~5.00 μg/kg，猪肉、牛肉、鸡蛋、虾肉、鸡皮、猪肝六种基质在5、10、50 μg/kg加标水平下，平均回收率为74.56%~119.28%，相对标准偏差（RSD，n=6）为0.91%~14.16%，回收率和精密度良好。该方法操作简单、准确、高效，稳定性好，适用猪肉、牛肉、鸡蛋、虾肉、鸡皮、猪肝中19种磺胺类药物残留的确证检测。

We developed a confirmatory detection method for 19 sulfonamide drug residues in foods of animal origin, which were double-purified using dialysis, followed by capture on a sulfonamide affinity column, and detected and analyzed using ultra-high performance liquid chromatography-tandem mass spectrometry. Samples were extracted with 80 % acetonitrile (0.2 % formic acid). Extracts were partially purified using dialysis, and sulfonamides were captured on a column (Speedy Prep®-Sulfa), then separated using an ACQUITY UPLC BEH C18 column. Gradient elution was carried out using a gradient of 0.2 % aqueous formic acid and methanol as the mobile phase. Mass spectrometry was performed using electrospray positive ion mode and multiple reaction monitoring modes. An external standard method was used for quantitative analysis. The results indicated that the sulfonamide capture column in this method could complete purification within 30 sec, and the entire pretreatment process required less than 10 min. The 19 sulfa drug concentrations were within their linear range (correlation coefficient r≥0.999 1), the limit of detection was 1.00~2.00 μg/kg, and the limit of quantification was 2.50~5.00 μg/kg. Pork, beef, eggs, shrimp, chicken skin, and pork liver were spiked at 5, 10, and 50 μg/kg, and average recovery ranged from 74.56% to 119.28%, with relative standard deviations (RSD, n=6) ranging from 0.91% to 14.16%, indicating good recovery and precision. The method described herein confers several advantages, including simple operation, high accuracy, excellent reproducibility, and suitability for quantifying sulfonamides in pork, beef, eggs, shrimp, chicken skin, and pork liver.

广东省粤港湾联合创新领域项目（2021A0505080003）；深圳市技术攻关重点项目（JSGG20191115141601721）