超高效液相色谱-串联三重四级杆质谱法测定富硒食品中的硒代氨基酸

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(r0.996),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。

Determination of selenoaminoacid in selenium enriched foods by ultra high performance liquid chromatography-tandem mass spectrometry

Objective To establish a method for determination of 4 kinds of Seleno amino acids in selenium enriched foods by ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods Three kinds of extraction methods for preparation of samples were discussed. A mixture of 0.1% formic acid (A) and acetonitrile (B) as mobile phases was used for Chromatographic separation of four kinds of selenium amino acids, including SeCys, SeMet, Se-(Methyl)seleno-L-cysteine and N-Acetyl-L-Selenomethionin. The four analysts were monitored with multiple reaction monitoring (MRM) mode. External standard method was employed to quantify. Results In oral liquid sample, all of the tested selenium amino acids showed good linear relationship (r>0.996). The average recoveries were between 89.0%-104.5% and the RSDs were less than 7% . Conclusion The present method is available for the sample with simple ingredient, nevertheless matrix effect is noticeable for the complex sample.