建立了一种柱后氨化-超高效液相色谱-串联质谱法(UPLC-MS/MS)测定牛奶和奶粉中三聚氰酸的分析方法.样品用5%三氯乙酸溶液提取,无需净化和浓缩,用Acquity UPLC HSS T3色谱柱(50 mm×2.1 mm,1.8 μm)进行分离,以乙腈和水作为流动相进行梯度洗脱,柱后氨化,电喷雾负离子(ESI-)模式电离,多反应监测(MRM)模式进行检测.结果表明:三聚氰酸在10.0～160.0 μg/L 范围内线性关系良好(r≥0.99).牛奶在0.05、0.10、0.20 mg/kg 的添加浓度的回收率为60%～118.5%,相对标准偏差(RSD,n=6)为8.2%～12.6%;奶粉在0.25、0.50、1.00 mg/kg 的添加浓度的回收率为88%～108%,RSD(n=6)为2.5%～5.7%.牛奶中方法的定量限(信噪比为10)为0.05 mg/kg,奶粉中为0.25 mg/kg.该方法快速、灵敏、准确,适合于牛奶、奶粉等乳及乳制品中三聚氰酸的快速、高灵敏度的分析检测.
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