建立了一种超高效液相色谱-串联质谱测定调制乳中磺胺嘧啶、磺胺甲基嘧啶和磺胺二甲基嘧啶残留的方法。调制乳经1％（ v／v）乙酸水溶液和甲醇提取、沉淀蛋白质，HLB 固相萃柱萃取净化处理后上机检测。采用 AC-QUITY UPLC HSS T3色谱柱，以0.1％（ v／v）甲酸水溶液和乙腈为流动相进行梯度洗脱，使用电喷雾离子源，在正离子模式下进行数据采集。采用基质标准样品添加法绘制标准曲线，外标法定量，方法的定量限为1μg／kg。在1~100μg／L范围内3种磺胺类药物标准曲线的线性关系良好（相关系数（R2）≥0.998）；在1、2和10μg／kg 3个加标水平下，方法的回收率为76.5％~101.9％，相对标准偏差为1.2％~12.4％。该方法简便、快速、实用、准确，各项技术指标满足国内外法规的要求，可用于调制乳中磺胺类药物残留的确证检测。
An ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS)method for the residue determination of sulfadiazine,sulfamerazine and sulfamethazine in modified milk was established. The modified milk samples were extracted and their protein pre-cipitated with water( containing 1%( v/v)acetic acid)and methanol. Then they were purified with an HLB solid phase extraction cartridge. The separation was performed on an ACQUITY UPLC HSS T3 column(100 mm×2.1 mm,1.8 μm)with a gradient system of water(containing 0.1%(v/v)formic acid)and acetonitrile as mobile phases at a flow rate of 0.3 mL/min,and detected by the MS in ESI+ mode. Standard curves were drawn by using matrix standard addi-tion method,and the external standard method was used for quantitative analysis. The limits of quantification were 1 μg/kg. The calibration curves for the three sulfa drugs were linear in the mass concentration range of 1-100 μg/L with R2≥0.998. The recoveries at the levels of 1,2,10μg/kg fortified samples ranged from 76.5% to 101.9% with the relative standard deviations of 1.2%-12.4%. The method is simple, rapid, accurate, and its performance can meet the requirements of the domestic and international legislations. It is suitable for the detection of sulfonamide residues in modified milk.
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