微波等离子体原子发射光谱分析富硒农产品中总硒  

Total selenium analysis in selenium-enriched agricultural products with microwave plasma atomic emission spectrometry

作　　者：江波[1] 陈林 JIANG Bo;CHEN Lin(School of Advanced Agriculture and Bioengineering,Yangtze Normal University,Fuling 408100,China;Institute of Chinese Materia Medica,Hunan Academy of Traditional Chinese Medicine,Changsha 410013,China)

机构地区：[1]长江师范学院现代农业与生物工程学院,重庆涪陵408100 [2]湖南中医药研究院中医研究所,湖南长沙410013

出　　处：《食品与发酵工业》2021年第20期247-252,共6页Food and Fermentation Industries

基　　金：国家自然科学基金项目(81603400);重庆市自然科学基金项目(cstc2018jcyjAx0594)。

摘　　要：建立微波等离子体原子发射光谱(microwave plasma atomic emission spectrometry,MP-AES)法测定富Se农产品中总Se含量的分析方法。采用微波消解对样品进行预处理,采用盐酸将Se(Ⅵ)还原为Se(Ⅳ),在多模式样品导入系统中使用L-半胱氨酸/酒石酸与消解溶液在线混合提高Se(Ⅳ)的还原效率,利用NaBH_(4)/NaOH将Se(Ⅳ)还原为H_(2)Se,采用MP-AES进行测定。选择196.026 nm为Se的分析波长,可避开光谱重叠干扰,利用快速线性干扰校正技术校正背景干扰。采用国家标准参考物质验证方法的准确性,总Se的测定结果与标准参考物质的参考值基本一致。Se的检出限(limit of detection,LOD)为0.58μg/L,不同富Se农产品中总Se的含量为0.11~1.84μg/g。MP-AES利用配备的N_(2)发生器产生大量N2取代气瓶或液体储存系统降低分析成本,提高分析效率,并且灵敏度和LOD俱佳。该方法可用于富Se农产品中总Se含量的准确测定。Analytical method was established for the determination of total selenium(Se)concentrations in selenium-enriched agricultural products using microwave plasma atomic emission spectrometry(MP-AES).After microwave digestion of selenium-enriched agricultural products,Se(Ⅵ)was reduced to Se(Ⅳ)by HCl.In the multimode sample introduction system(MSIS),the reduction efficiency of Se(Ⅵ)was improved by on-line mixing of L-cysteine/tartaric acid with the sample solution,Se(Ⅳ)was reduced to H_(2)Se using NaBH_(4)/NaOH,and MP-AES was used for determination.And 196.026 nm was selected as the analysis wavelength of Se to avoid spectral interference.The fast-linear interference correction(FLIC)model was used to correct the background interference.The national standard reference materials were used to verify the accuracy of the method,and the determination results of total Se were consistent with the certified value of the standard reference materials.Furthermore,the limit of detection(LOD)was 0.58μg/L,and the total Se content in different selenium-enriched agricultural products was between 0.11-1.84μg/g.In addition,MP-AES reduced the analytical cost and improved the analytical efficiency by replacing bottles or liquid storage systems with abundantly available nitrogen from a generator.With good sensitivity and LOD,this method can be used for the accurate determination of total Se concentrations in selenium-enriched agricultural products.

关 键 词：富硒农产品 总硒 微波等离子体原子发射光谱 多模式样品导入系统 快速线性干扰校正 

分 类 号：O657.3[理学—分析化学] TS207.3[理学—化学]