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吕亚宁, 宋伟, 沈贵兰, 等. 高效液相色谱-电感耦合等离子体质谱法同时测定果汁饮品中砷、硒与铬元素的无机形态[J]. 分析测试学报, 2018,37(9):1087-1091.
Simultaneous Determination of Inorganic Speciations of As,Se and Cr in Juice Drinks by High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry[J]. 2018,37(9):1087-1091.
建立了高效液相色谱(HPLC)与电感耦合等离子体质谱(ICP-MS)联用技术同时测定果汁饮品中Cr(Ⅵ)、Cr(Ⅲ)、As(Ⅲ)、As(Ⅴ)、Se(Ⅳ)和Se(Ⅵ)6种元素无机形态的方法。样品经超声提取后,加入EDTA溶液,采用C8色谱柱分离,以0.1 mmol/L四丁基氢氧化铵+0.1 mmol/L乙酸铵+10%甲醇为流动相等度洗脱,ICP-MS测定。选用DRC模式消除干扰,保证了测定的准确性。上述6种元素无机形态的方法检出限分别为0.34、0.20、0.50、0.40、0.82、0.90 μg/L,回收率为79.5%~112%,相对标准偏差(RSD)小于5.0%。应用该法检测实际样品,其中苹果汁未检出该6种形态;蓝莓汁检出Cr(Ⅲ)、Se(Ⅳ),含量分别为0.007、0.015 mg/kg;杂粮汁检出3种形态,含量为0.008~0.034 mg/kg。
A high performance liquid chromatography(HPLC)coupled with inductively coupled plasma mass spectrometric(ICP-MS) method was developed for the determination of six kinds of inorganic elements,including Cr(Ⅵ),Cr(Ⅲ),As(Ⅲ),As(Ⅴ),Se(Ⅳ)and Se(Ⅵ)in juice drinks.After ultrasonic extraction,the samples were added with EDTA solution,separated with a C8 column using 0.1 mmol/L tetrabutyl ammonium hydroxide,0.1 mmol/L ammonium acetate and 10% methanol as mobile phases,and then determined by ICP-MS.The DRC mode was used to eliminate the interference and ensure the accuracy of determination.The detection limits for the 6 element speciations were 0.34,0.20,0.50,0.40,0.82 and 0.90 μg/L,respectively.The recoveries for the analytes were between 79.5% and 112% with the relative standard deviations(RSDs)(n=6)less than 5.0%.Using this method,six inorganic speciations were undetected in apple juice,while Cr(Ⅲ)and Se(Ⅳ)were detected in blueberry juice with contents of 0.007 mg/kg and 0.015 mg/kg,respectively,and 3 element speciations were detected in cereals juice with contents of 0.008-0.034 mg/kg.
高效液相色谱-电感耦合等离子体质谱法元素无机形态果汁饮料砷硒铬
high performance liquid chromatography-inductively coupled plasma mass spectrometryinorganic morphology of elementsjuice drinksAsSeCr
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