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目的建立一种用于检测富硒食品中4种硒代氨基酸的超高效液相色谱-串联质谱法。方法考虑3种样品前处理方法的影响,采用0.1%的甲酸(A)和乙腈(B)二元流动相体系对N-乙酰-L-硒代蛋氨酸、Se-(甲基)硒基-L-半胱氨酸、硒代蛋氨酸和硒代胱氨酸等4种硒代氨基酸进行色谱分离。采用多反应监测模式(multiple reaction monitoring,MRM)进行监测,基质匹配外标法进行定量。结果口服液中,4种硒代氨基酸的线性关系良好(r>0.996),平均回收率范围为89.0%~104.5%,相对标准偏差均小于7%。结论该方法对简单基质的样品中硒代氨基酸的测定结果准确可靠,但基质效应较为明显。
OBJECTIVE To establish a ultra performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method for the determination of four seleno amino acids in selenium-enriched foods. Methods Considering the influence of three sample pretreatment methods, 0.1% formic acid (A) and acetonitrile (B) binary mobile phase system were used to evaluate the effect of N-acetyl-L-selenomethionine, Se- - Cysteine, selenomethionine and selenocystine and other four seleno amino acids were separated by chromatography. Multiple reaction monitoring (MRM) was used for monitoring and matrix matching for external standard quantification. Results The oral liquid showed good linearity (r> 0.996) for the four selenoamino acids. The average recoveries ranged from 89.0% to 104.5% with relative standard deviations less than 7%. Conclusion This method is accurate and reliable for the determination of seleno-amino acids in simple matrix samples, but the matrix effect is obvious.