分子荧光紧密内插法快速测定饲料中的硒
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摘要
为创建一种新型测定饲料中硒的方法,用微波消解样品,在酸性条件下,硒与2,3-二氨基萘(DAN)反应生成具有强荧光特性的4,5-苯并苤硒脑,其荧光强度与硒的含量成正比,以此用分子荧光紧密内插法测定饲料中的硒。结果表明:最佳测定条件为pH 1.5、DAN试剂4.00 mL、EDTA混合液20.00 mL、水浴时间6 min。饲料样品中硒的含量大于5.83 mg/kg,加标回收率大于92%。本方法具有快速简便、成本低廉、样品用量少、消解完全、无需测定空白和绘制标准曲线的优点,有较强的推广应用价值。
In order to establish a new method for the determination of selenium in feed,the sample was digested by microwave method,under acidic conditions,selenium reacts with 2,3-diaminonaphthalene(DAN)to produce a strong fluorescence characteristic of 4,5-benzobenzelenol,the fluorescence intensity was proportional to the content of selenium,the determination of selenium in feed by molecular fluorescence compact interpolation method.The results showed that the optimum measurement condition pH was 1.5,the DAN reagent dosage was 4.00 m L,EDTA mixture was 20.00 mL and the bath time was 6 min.The content of selenium in feed samples was greater than 5.83 mg/kg and the standard recovery was greater than 92%.This method was fast and simple,low cost,less sample usage and complete dissolution.It does not need to measure blank solution and draw standard curve,so it has strong value of popularization.
In order to establish a new method for the determination of selenium in feed,the sample was digested by microwave method,under acidic conditions,selenium reacts with 2,3-diaminonaphthalene(DAN)to produce a strong fluorescence characteristic of 4,5-benzobenzelenol,the fluorescence intensity was proportional to the content of selenium,the determination of selenium in feed by molecular fluorescence compact interpolation method.The results showed that the optimum measurement condition pH was 1.5,the DAN reagent dosage was 4.00 m L,EDTA mixture was 20.00 mL and the bath time was 6 min.The content of selenium in feed samples was greater than 5.83 mg/kg and the standard recovery was greater than 92%.This method was fast and simple,low cost,less sample usage and complete dissolution.It does not need to measure blank solution and draw standard curve,so it has strong value of popularization.
引文
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[12]Serra A M,Estela J M,Coulomb B,et al.Solid phase extractionMultisyringe flow inject system for the spectrophotometric determination of selenium with 2,3-diaminonaphthalene[J].Talanta,2010,81(1):572~577.
[2]高向阳,王方方.化学发光紧密内插法快速测定饲料中的微量铬[J].饲料工业,2017,38(20):50~54.
[3]高向阳,杨梦柯.分子荧光紧密内插法快速测定饲料中的铝[J].饲料研究,2017,21:42~46,49.
[4]候晓芳,迟忠云,王悦霞.氢化物发生原子吸收法测定保健食品中硒含量[J].海峡预防医学杂志,2009,1:55~56.
[5]可成友,朱孔儒,张译,等.火焰原子吸收分光光度计对纯化水硒含量的测定[J].当代化工,2015,44(6):1432~1437.
[6]王永华.食品分析.第二版[M].北京:中国轻工业出版社,2016.167.
[7]卫生部.GB5009.93-2017[S].食品安全国家标准食品中硒的测定.北京:中国标准出版社,2017.
[8]杨雁玲.微波消解DAN荧光法测定饲料中的微量硒[J].中国饲料,2007,18:35~37.
[9]赵艳.分子荧光测定富硒盐中的硒含量[J].广州化工,2016,44(17):133~134.
[10]钟秀倩,钟俊辉.微量元素与人体健康[J].现代预防医学,2015,34(1):61~63.
[11]周跃花,杨菊香,王艳.微波消解分子荧光法测定茶叶中硒的含量[J].安徽农业科学,2009,37(22):351~353.
[12]Serra A M,Estela J M,Coulomb B,et al.Solid phase extractionMultisyringe flow inject system for the spectrophotometric determination of selenium with 2,3-diaminonaphthalene[J].Talanta,2010,81(1):572~577.