离子色谱-氢化物发生-原子荧光光谱(IC-HG-AFS)联用技术检测胶州湾海产品中硒的赋存形态  

Selenium speciation analysis in aquatic products of Jiaozhou Bay by ion chromatographic hydride generation- atomic fluorescence spectrometry

作　　者：韩婷婷[1,2] 崔鹤[2] 宋田[3] 姬泓巍[1] 李慧新[2] 朱倩林[1] 蔡峰[2] 张涛[2] 

机构地区：[1]中国海洋大学化学化工学院,山东青岛266100 [2]山东出入境检验检疫局检验检疫技术中心,山东青岛266002 [3]燕山大学理学院,河北秦皇岛066004

出　　处：《食品工业科技》2016年第18期81-84,99,共5页Science and Technology of Food Industry

基　　金：国家重大科学仪器设备开发专项(2012YQ090229)

摘　　要：建立了离子色谱-氢化物发生-原子荧光光谱联用技术（IC-HG-AFS）测定胶州湾海产品中4种硒形态的方法。研究了色谱柱、流动相、提取剂、提取温度及其仪器条件等对硒荧光信号值的影响。试样用1.5 mol/L的氢氧化钾溶液作提取液,采用AS11-HC（250 mm×4.1 mm,5.0μm）阴离子色谱柱,20 mmol/L碳酸氢钠溶液/2%乙腈为流动相,1.0 m L/min流速,可在8 min内同时分离检测硒代胱氨酸（Se Cys）、硒代蛋氨酸（Se Met）、亚硒酸根Se（Ⅳ）和硒酸根Se（Ⅵ）。当4种形态的质量浓度范围为0~100μg/L时,各形态均得到良好的线性关系,线性相关系数均大于0.996,各形态的检出限分别为Se Cys 1.53μg/L,Se Met 1.72μg/L,Se（Ⅳ）0.30μg/L,Se（Ⅵ）1.06μg/L,相对标准偏差RSD均小5%（n=6）,在最佳条件下,应用该方法测定了水产品中的硒形态,4种硒形态化合物加标回收率在86.1%~105.3%之间。该方法测定海产品中的硒形态准确、可靠、简便灵敏,为科学有效地评价海产品质量和开展风险评估提供技术支撑。A sensitive analytical method was developed for speciation of aquatic products of Jiaozhou Bay by ion chromatography hydride generation - atomic fluorescence spectrometry （ IC - HG - AFS）, Learning the mobile phases, extraction reagents, extraction temperature and instrumental conditions was influence for selenium fluorescence signal value.The sample was extracted by the 1.5 mol/L Kalium hydroxide solution.Using the AS11- HC（250 mm ×4.t mm,5.0μm）anion column,20 mmol/L Sodium hydrogen carbonate solution,2% acetonitrile mobile phase, 1.0 mL/min velocity of flow. It could be separated simultaneously in 8 minutes, detecting the Selenocystine（ SeCys）, Selenomethionine （ SeMet）, Se （ Ⅳ ） and Se （ Ⅵ ）. On the optimized conditions, linear relationships between values of fluorescence intensity and mass concentration of selenium species were found in the same range of 0~ 100 μg/L,with the correlative coefficients more than 0.996.The detection limits（3 s/k）of SeCys, SeMet, Se （ Ⅳ ）, Se （ Ⅵ ） were 1.53,1.72,0.30,1.06 μg/L, respectively, and the relative standard deviations （ n = 6）for the selenium species were all less than 5%.Applying the present procedure to the speciation analysis of selenium in aquatic products, the spiked recoveries from 86.1% to 105.3% were obtained. The method for the determination of selenium species in aquatic products was accurate, reliable, simple and sensitive, and effectiveness for the scientific evaluation of the quality of aquatic products and to provide technical support for conduct risk assessments.

关 键 词：离子色谱 氢化物发生原子荧光 胶州湾 海产品 硒形态 

分 类 号：TS207.3[轻工技术与工程—食品科学]