【摘要】 建立了高效液相色谱-电喷雾质谱联用技术（HPLC-ESI-MS）检测蚯蚓体内硒代氨基酸的分析方法.采用振荡超声辅助酶解法提取蚯蚓（赤子爱胜蚓（Eisenia fetida））体内的硒代蛋氨酸（SeMet）和甲基硒代半胱氨酸（MeSeCys）.用HPLC-ESI-MS正离子多反应离子监测模式（MRM）对这两种硒代氨基酸进行分离检测,外标法定量.SeMet和MeSeCys在4—600 ng·mL^-1有良好的线性关系,线性相关系数R²均大于0.9999.SeMet和MeSeCys的方法检出限分别为0.49μg·g^-1和0.67μg·g^-1.样品加标回收率在81.1%—112.4%之间,并且相对标准偏差RSD均小于3.1%.本方法不需要柱前衍生化,增加反向气等繁琐操作,简单快速的实现对两种硒代氨基酸的分离检测.更多还原

【Abstract】 A high performance liquid chromatography-electrospray ionization-mass spectrometry（HPLC-ESI-MS） method was developed for the determination of the seleno amino acids in earthworms. Selenomethione（SeMet） and methylselenocysteine（MeSeCyS） were extracted from earthworms by oscillating and ultrasound assisted enzymatic hydrolysis. These two seleno amino acids were isolated and determined by HPLC-ESI-MS using external standard method. Then the positive ion and multiple reaction monitoring（MRM） was applied and operated. The results indicated that both SeMet and MeSeCys had a good calibration curve in a range of 4—600 ng·mL^-1, with R² > 0.9999. The method detection limits of SeMet and MeSeCys were 0.49 μg·g^-1 and 0.67 μg·g^-1, respectively. The recoveries of standard addition were 81.1%—112.4%, with RSD values less than 3.1%. This detection method was preferred over others as it had eliminated the need for more cumbersome procedures, such as pre-column derivatization and increased the opposite direction gas.更多还原