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目的建立超高效液相色谱-串联质谱法测定硒代蛋氨酸(Se Met)的方法,并用于测定牛奶中游离Se Met。方法在Acquity UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm)上以水∶乙腈∶甲酸(95∶5∶0.1,V/V)为流动相,流速0.3 m L/min,柱温40℃,分析时间2.5 min,在电喷雾-正离子电离源上以多反应监测模式分析Se Met,用于定量分析的离子反应为m/z 198.0→181.1。结果 Se Met线性范围为0.5~100 ng/m L,方法的定量下限为0.5 ng/m L。Se Met批内准确度在97.6%~100.6%,批间准确度在97.7%~99.2%,批内精密度在0.53%~4.49%,批间精密度在1.03%~4.54%。结论 UPLC-MS/MS法具有特异性好、灵敏度高、分析速度快和准确可靠的优点,适用于牛奶中游离Se Met的定量测定。
Objective To establish a method for the determination of Se Met in milk by ultra performance liquid chromatography-tandem mass spectrometry. Methods The mobile phase was eluted at a flow rate of 0.3 m L / min on a Acquity UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 μm) using water: acetonitrile: formic acid (95: 5: 0.1 V / V) ℃, and the analysis time was 2.5 min. Se Met was analyzed by electrospray-positive ionization (ESI) on a multi-reaction monitoring mode. The ion reaction used for quantitative analysis was m / z 198.0 → 181.1. Results Se Se linear range of 0.5 ~ 100 ng / m L, the method of quantitative limit of 0.5 ng / m L. The accuracy of Se Met was 97.6% ~ 100.6%, the accuracy of inter-assay was 97.7% ~ 99.2%, the precision of batch was 0.53% ~ 4.49%, and the precision of batch was 1.03% ~ 4.54%. Conclusion The UPLC-MS / MS method has the advantages of good specificity, high sensitivity, fast analysis speed and accuracy and reliability. It is suitable for the quantitative determination of free Se Met in milk.