超声辅助酶法提取-液相色谱-原子荧光光谱法测定富硒黑木耳中硒形态

Determination of Selenium Speciation in Se-enriched Auricularia Auricula by Atomic Fluorescence Spectroscopy with Ultrasonic-Assisted Enzymatic Extraction

建立了富硒黑木耳中硒代胱氨酸、硒代半胱氨酸、亚硒酸、硒蛋氨酸、硒酸5种硒形态的液相色谱-原子荧光光谱分析方法。通过链酶蛋白酶E酶解,结合超声提取后,选取Hamilton PRP-X100离子交换色谱柱(250 mm×4.1 mm,10μm),40 mmol/L的磷酸氢二铵为流动相,在16 min内,5种硒形态完全达到基线分离。5种硒形态在线性范围内相关系数R为0.9990~0.9999;加标回收率为76.1%~108%;检出限分别为硒代胱氨酸0.35μg/L、甲基-硒代半胱氨酸0.46μg/L、亚硒酸0.26μg/L、硒代蛋氨酸0.64μg/L、硒酸3.06μg/L;方法应用于富硒黑木耳中硒形态的分析,精密度高、重现性好、方法稳定、准确可靠,是测定富硒黑木耳中硒形态含量的有效方法。

A method for the determination of selenocystine,selenocysteine,selenious acid,selenomethionine and selenic acid in se-enriched auricularia auricula by liquid chromatography combined atomic fluorescence spectrometry was established.After enzymolysis of strepase E with the ultrasonic extraction,the Hamiltonian PRP-X100 ion exchange column(250 mm×4.1 mm,10μm)and the mobile phase of 40 mmol/L diammonium hydrogen phosphate and 0.4%potassium iodide were selected.Within 16 minutes,the five selenium speciation were completely separated at baseline.The correlation coefficient R of the five selenium speciation was 0.9990~0.9999,and the recoveries were 76.1%—108%The detection limits of selenocystine,methyl selenocysteine,selenious acid,selenomethionine and selenic acid were 0.35μg/L,0.46,0.26,0.64,3.06,respectively.The method was applied to the determination of selenium speciation in Se-enriched auricularia auricula in linear range.