HPLC-ICP-MS在线联用分析食品中无机硒和硒氨基酸的形态  

Simultaneous quantification of the speciation of inorganic selenium and Se amino acids in food by high performance liquid chromatography combined with inductively coupled plasma mass spectrometry

作　　者：熊珺 覃毅磊 龚亮 赖毅东 

机构地区：[1]广东省东莞市质量监督检测中心,广东东莞523808 [2]广东省东莞市食品药品检验所,广东东莞523109

出　　处：《食品工业科技》2017年第4期67-72,共6页Science and Technology of Food Industry

基　　金：广东省质量技术监督局科技项目(2013ZS01)

摘　　要：以亚硒酸盐(Se(Ⅳ))、硒酸盐(Se(Ⅵ))、硒胱氨酸(Se Cys_2)、硒蛋氨酸(Se Met)、甲基硒代半胱氨酸(Me Se Cys)和硒代乙硫氨酸(Se Et)为硒形态的目标分析物,采用Dionex Ion Pac AS11色谱柱(250 mm×4.0 mm)为分离柱,通过优化流动相的p H、浓度、甲醇含量、流速和色谱柱的柱温等因素对六种目标硒形态分离及不同提取方法对目标分析物提取效率的影响,建立了高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)在线联用同时测定食品中无机硒和硒氨基酸的分析方法。Me Se Cys、Se Met、Se Et、Se(Ⅳ)、Se Cys_2和Se(Ⅵ)的检出限分别为0.25、0.20、0.35、0.15、0.30、0.15μg Se/L;Me Se Cys和Se Cys_2的线性范围为2.0~2500μg Se/L,Se(Ⅳ)和Se(Ⅵ)线性范围为1.2~1200μg Se/L,Se Met和Se Et的线性范围分别是1.5~1500μg Se/L和2.2~2200μg Se/L,各硒形态的线性相关系数均不少于0.9997。将该方法应用于食品中硒形态的分析,其加标回收的回收率为80.8%~106.7%,相对标准偏差(RSDs,n=3)为4.7%~9.6%。方法具有操作简单、方便快速、灵敏度高和环境友好等优点,可满足食品中硒形态定量分析。A new method based on high performance liquid chromatography combined with inductively coupled plasma mass spectrometry（ HPLC- ICP- MS） for selenium speciation of inorganic selenium and Se amino acids has been developed. The different parameters affecting extraction efficiency and the retention behaviors of six target selenium species including the effect of p H and concentration of mobile phase,methanol content,flow rate and column temperature had been studied. Under the optimal condition of the mobile phase of 7.5 mmol / L diammonium phosphate buffer solution（ p H11.0） with flow rate of0.60 m L / min,six target selenium species including Se O_3～（2-）（ Se（ IV））,Se O_4～（2-）（ Se（ Ⅳ））,L- Selenocystine（ Se Cys2）,DLSelenomethionine（ Se Met）,Se- methylseleno- L- Cysteine（ Me Se Cys）,Seleno- D,L- Ethionine（ Se Et） were separated completely.The limits of detection for the target compounds were varied from 0.15 to 0.35 μg Se / L and the calibration curves were linear in the range of 2.0～2500 μg Se / L for Me Se Cys and Se Cys2,1.2～1200 μg Se/L for Se（ Ⅳ） and Se（ Ⅵ）,1.5～1500 μg Se / L for Se Met and 2.2～2200 μg Se / L for Se Et with good correlation coefficient（ R2≥0.9997）.The recoveries at three spike levels ranged from 80.8% to 106.7% with the relative standard deviations（ RSDs,n = 3） of 4.7～9.6%.The method was found to be simple,rapid,efficient and inexpensive,and provided an accurate and sensitive detection platform for elemental speciation in food samples.

关 键 词：无机硒 硒氨基酸 高效液相色谱-电感耦合等离子体质谱 食品 

分 类 号：TS207.3[轻工技术与工程—食品科学]