柱前衍生高效液相色谱荧光检测法测定奶粉中L-硒-甲基硒代半胱氨酸

摘要

A method for the determination of L-Se-methylselenocysteine in milk powder by HPLC with fluorescence detection and precolumn derivatization was established.The milk powder was treated with acetonitrile and solid phase extraction（SPE） for cleaning up prote%建立了硒营养强化奶粉中L-硒-甲基硒代半胱氨酸含量柱前衍生高效液相荧光检测测定方法。奶粉样品经乙腈沉淀蛋白,上固相萃取柱处理后,与邻苯二甲醛和3-巯基丙酸进行衍生化反应。然后采用Diamonsil C18色谱柱（250mm×4.6mm,5μm）,醋酸盐缓冲液-乙腈-甲醇为流动相,流速为1mL·min-1,柱温40℃,荧光检测波长λex=343nm,λem=454 nm,进样量20μL,以三（羟甲基）氨基甲烷为内标进行测定。在1.3-22.0μg·mL-1浓度范围内与相对峰面积呈良好的线性关系,回归方程为：