超声辅助提取-HPLC-ICPMS联用分析食品中水溶性铬价态
目的 建立一种超声辅助提取-高效液相色谱分离-电感耦合等离子体质谱仪联用法(HPLC-ICP/MS)测定食品中水溶性铬价态分析方法。方法 样品经EDTA-硝酸铵混合溶液提取后,含蛋白质的样品加入铁氰化钾和乙酸锌溶液沉淀蛋白质,0.45μm微孔滤膜过滤后备用。样品经离子交换柱分离,ICP/MS检测。结果 Cr(III)和Cr(VI)在0.5 ng/mL～50 ng/mL的范围内呈线性关系,大米和鸡蛋样品在0.025mg/kg,0.05mg/kg和2.0mg/kg添加水平下的回收率为62%~117.9%；土豆在0.025mg/kg,0.05mg/kg和1.0mg/kg添加水平下回收率为80.2%~118.2%；牛奶在0.025mg/kg,0.05mg/kg和0.6 mg/kg添加水平下回收率为64.5%~106.5%,日内相对标准偏差小于8%,日间相对标准偏差小于10%；两种价态的铬的检出限均为10 μg/kg。结论 该方法快速、准确、灵敏, 适合用于多种食品中可溶性铬价态分析检测。
Objective To determination of method for valence state analysis of water soluble chromium in foods by HPLC-ICP/MS used ultrasound assisted extraction. Methods Samples were extracted with EDTA-ammonium nitrate mixture solvent. Protein were precipitated with potassium ferricyanide and zinc acetate solution for samples containing protein. The extract was separated by ion exchange column and was test by ICP/MS after microfiltration membrane filtration. Results There are linear relationship in the range of 0.5 ng/mL to 50 ng/mL for both Cr(III) and Cr(VI). The recoveries were range from 62% to 117.9% for the mice and eggs with 3 spiked levers of 0.025mg/kg，0.05mg/kg and 2.0mg/kg. The recovery was range from 80.2% to 118.2% for the potato with 3 spiked levers of 0.025mg/kg，0.05mg/kg and 1.0mg/kg. The recvery was range from 64.5% to 106.5% for the milk with 3 spiked levels 0.025mg/kg，0.05mg/kg and 0.6 mg/kg. The interday relative standard deviations (RSDs) were less than 8% (n=6) and the intraday R.S.D. were less than 10%(n=6). The limits of detection (LOD) for the Cr(III) and Cr(VI) were 10 μg/kg. Conclusion The proposed method is fast, accurate and sensitive, which is suitable for the analysis and determination of soluble chromium in various foods.
标题：超声辅助提取-HPLC-ICPMS联用分析食品中水溶性铬价态
英文标题：Analysis of water soluble chromium valence state in food by HPLC-ICP/MS with ultrasonic assisted extraction
作者：
葛晓鸣 宁波检验检疫科学技术研究院
冯睿 宁波检验检疫科学技术研究院
孙骥 宁波检验检疫科学技术研究院
叶海雷 宁波检验检疫科学技术研究院
金婉芳 宁波检验检疫科学技术研究院
陈先锋 宁波检验检疫科学技术研究院
马明 宁波检验检疫科学技术研究院
中文关键词:HPLC-ICP/MS,铬,价态分析,
英文关键词:HPLC-ICP/MS,Chromium,valence state analysis,,
发表日期：2018-08-15
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