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氢化物原子荧光光谱法测定乳粉中总硒含量

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文章建立了微波消解-氢化物原子荧光光谱法测定乳粉中总硒含量的分析方法.利用6 mol/L的盐酸进行处理,反应温度为80℃,反应时间为20 min,以3%(V/V)的盐酸和1.0 g/100 mL硼氢化钾为还原剂和载流,测定含有硒酸、亚硒酸、硒代胱氨酸、硒代蛋氨酸、甲基硒半胱氨酸5种不同形态硒乳粉中总硒含量.结果表明,在最优试验条件下,硒含量在0~10 μg/L范围内线性关系良好,线性相关系数大于0.9998,检出限为0.001 mg/kg.对国家标准物质乳粉中硒含量进行测定,其检测结果在参考值范围内.在低、中、高3个水平下的加标回收率为98.2%~109%,RSD值为1.49%~5.29%.本方法适用于含有不同硒形态乳粉中总硒含量的检测.
Determination of total selenium content in milk powder by hydride atomic fluorescence spectrometry
A method was established for the determination of total selenium in milk powder by microwave digestion-hydride atomic fluorescence spectrometry.Using 6 mol/L hydrochloric acid for treatment,the reaction temperature was set at 80 ℃ and the reaction time was 20 minutes,with 3%(V/V)hydrochloric acid and 1.0 g/100 mL potassium borohydride as the reducing agent and carrier,the total selenium content in the milk powder containing selenium acid,selenious acid,selenocysteine,selenomethionine,and methylselenocysteine in five different forms was deter-mined.The experimental results showed that under the optimal experimental conditions,the selenium content showed good linear relationship in the range of 0-10 μg/L with the linear correlation coefficient(was)greater than 0.9998,the detection limit was 0.001 mg/kg.The selenium con-tent in milk powder of the national standard substance was determined,and the detection results were within the range of reference values.and the standard recoveries were in the range of 98.2%-109.0%at low,medium and high levels,and RSD values were in the range of 1.49%-5.29%.This method is applicable to the detection of total selenium content in milk powder containing different selenium forms.

milk powdermicrowave digestionatomic fluorescence spectrometryselenic acidselenite acid

张寒霜、赵发、韩晓晓、冉佼艳、董瑞、于文江、高喜凤、李芳芳、刘艳明

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山东省食品药品检验研究院,济南 250101

产业技术基础公共服务平台,济南 250101

乳粉 微波消解 原子荧光光谱法 硒酸 亚硒酸

山东省市场监督管理局科研项目

SDSJKJ202310

2024

中国乳品工业
黑龙江乳品工业技术开发中心,中国乳制品工业协会

中国乳品工业

CSTPCD北大核心
影响因子:0.41
ISSN:1001-2230
年,卷(期):2024.52(9)
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