摘要
建立了测定赣南脐橙中硒代胱氨酸(SeCys_(2))、甲基-硒代半胱氨酸(MeSeCys)和硒代蛋氨酸(SeMet)的UPLC-Q-TOF-MS分析方法.样品通过超声水提取,选取AccQ·Tag^(TM)氨基酸色谱柱(3.9 mm×150 mm),以水-甲醇(90∶10)为流动相进行分离,经电喷雾离子源(ESI)正离子化后,采用多反应离子监测方式(MRM)和外标法定量.实验结果表明,SeCys_(2)、MeSeCys、SeMet在5 ng/mL~100 ng/mL范围线性良好,相关系数R^(2)≥0.997;3种硒代氨基酸的加标回收率在78.8%~92.2%之间,相对标准偏差在2.1%~7.5%之间;SeCys_(2)、MeSeCys、SeMet的检出限分别为6 ng/mL、10 ng/mL、1 ng/mL.因此,该方法可以用于富硒脐橙中3种硒代氨基酸的准确和高效检测.
A ultra high performance liquid-time of flight high resolution mass spectrometry method was established for the determination of selenocystine(SeCys),Methyl-selenocysteine(MeSeCys)and selenomethionine(SeMet)in Gannan navel orange.The samples were extracted by sonicated water,selected AccQ·Tag^(TM) amino acid chromatographic column(3.9 mm×150 mm),were separated by the mobile phase of water-methanol(90:10),with the positive ionization by electrospray ion source(ESI),adopted multi-reaction ion monitoring method(MRM),and quantitated with external standard method.The experimental results showed that the good linearity of SeCys_(2),MeSeCys and SeMet ranged from 5 to 100 ng/mL,with the correlation coefficient of R^(2)≥0.997;the add standard recovery rate of three selenoamino acids ranged from 78.8%to 92.2%,with the relative standard deviation from 2.1% to 7.5%;the detection limits of SeCys_(2),MeSeCys and SeMet respectively were 6,10 and 1 ng/mL.Herein,the method could be used for the accurate and efficient detection of three selenoamino acids in Gannan selenium enriched navel orange.
作者
傅世利
兰费香
符娜妮
杨志燕
李勋
薛珺
FU Shili;LAN Feixiang;FU Nani;YANG Zhiyan;LI Xun;XUE Jun(School of Chemistry and Chemical Engineering,Gannan Normal University,Ganzhou 341000,China)
出处
《赣南师范大学学报》
2022年第3期49-52,共4页
Journal of Gannan Normal University
基金
国家自然科学基金资助项目(21964003)
江西省教育厅科学技术研究项目(GJJ201430)
赣州市重点研发项目(202101075041)。