超声-微波协同提取-高效液相色谱-电感耦合等离子体质谱法测定莓茶中的硒形态  

Determination of Selenium Species in Ampelopsis Grossedentata Tea by Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry After Ultrasonic-Microwave Synergistic Extration

作　　者：王贤波[1] 刘超[1] 叶生月 张乐[1] 余继忠[1] 刘军波[1] 余霞奎[1] WANG Xianbo;LIU Chao;YE Shengyue;ZHANG Le;YU Jizhong;LIU Junbo;YU Xiakui(Experimental Center of Hangzhou Academy of Agricultural Sciences,Hangzhou 310024,China;Tonglu County Agricultural Industrialization Development Service Centers,Hangzhou 311500,China)

机构地区：[1]杭州市农业科学研究院实验中心,浙江杭州310024 [2]桐庐县农业产业化发展服务中心,浙江杭州311500

出　　处：《食品科技》2023年第5期272-277,共6页Food Science and Technology

基　　金：杭州市农科院科技创新与示范推广基金项目(2020HN CT-26)。

摘　　要：建立了高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)检测莓茶中硒代半胱氨酸(SeCys)、甲基-硒代半胱氨酸(MeSeCys)、亚硒酸根[Se(Ⅳ)]、硒代蛋氨酸(SeMet)、硒酸根[Se(Ⅵ)]和硒代乙硫氨酸(SeEt)的方法。样品采用蛋白酶E超声-微波协同提取50 min,经C_(18)色谱柱分离,以30.0 mmol/L磷酸氢二铵、2.0 mmol/L四丁基溴化铵、2.0%甲醇为流动相(pH7.4),碰撞反应池技术消除多原子离子干扰,ICP-MS检测^(78)Se同位素,在14 min内可完全分离检测6种硒形态。在1~100μg/L范围内,各硒形态线性关系良好,相关系数r>0.999,方法检出限为0.05~0.14μg/L。加标回收率为85.3%~104.5%,相对标准偏差为1.6%~6.1%,研究发现莓茶中主要硒形态为Se Met。该方法简单、快速、灵敏度高,可用于莓茶中硒形态分析。To establish a method for determination of 6 different forms of selenium [Selenocysteine(SeCys),methyl selenium generation L-cysteine(MeSeCys),selenium acid radical(Se Ⅵ),selenomethionine(SeMet),selenium acid group(Se Ⅵ) and Seleno-D,L-ethionine(SeEt)] in Ampelopsis grossedentata tea samples by high liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP-MS).The samples were hydrolyzed by adding pronase E and extracted by ultrasonic-microwave synergistic for 50 min.Selenium species were separated by C18 chromatographic column using 30 mmol/L diammonium phosphate,2.0 mmol/L tetrbutyl ammonium bromide,and 2% methanol as mobile phase(pH7.4).Collision cell technology was adopted to eliminate the interference of polyatomic ions,and isotope ~(78)Se was detected by ICP-MS.The six species were completely separated within 14 min.The linear correlation coefficients(r) were all above 0.999 in the range of 1-100 μg/L.The limits of detection of the method were 0.05-0.14 μg/L.The recoveries were between 85.3%-104.5%,and the relative standard deviations were 1.6%-6.1%.The main form of selenium in Ampelopsis grossedentata tea is SeMet.The proposed assay is simple,rapid,and sensitive,which can be used for speciation analysis of selenium in Ampelopsis grossedentata tea.

关 键 词：高效液相色谱-电感耦合等离子体质谱 莓茶 硒形态 超声-微波协同 

分 类 号：TS207.3[轻工技术与工程—食品科学]