电感耦合等离子体质谱法同时测定植物类新食品原料中14种无机元素
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摘要
0.500 0g样品经硝酸3mL、过氧化氢2mL消解后,采用电感耦合等离子体质谱法同时测定样品溶液中Na、Mg、Ca、Al、Cu、Zn、Fe、Mn、Se、Pb、Cd、As、Hg和Cr的含量。采用0.5%(体积分数)硝酸的基体酸度增强分析元素的信号强度;在两次测试之间用100μg·L-1 Au-5%(体积分数)硝酸溶液清洗仪器,降低Hg的吸附效应;利用甲烷碰撞动态反应池技术消除了分析过程中的质谱干扰,选择Sc、Y、In、Bi为内标元素校正基体效应。14种元素的质量浓度在一定范围内与信号强度呈线性关系,检出限(3s)在0.003~0.039μg·L~(-1)之间。方法用于分析国家标准物质GBW 10027,各元素测定值与认定值相符,测定值的相对标准偏差(n=6)在1.6%~14%之间。
The sample(0.500 0 g)was digested with 3 mL of nitic acid and 2 mL of hydrogen peroxide,and Na,Mg,Ca,Al,Cu,Zn,Fe,Mn,Se,Pb,Cd,As,Hg,Cr in the sample solution were determined by ICP-MS.Acidity of φ 0.5% HNO_3 of the sample solution was adopted to enhance signal intensities of the 14 elements.The instrument was washed with 100μg·L~(-1) Au in φ 5% HNO_3 solution between 2 determinations to lower the adsorption effect of Hg.Mass spectral interference was eliminated using DRC mode with CH_4 as reaction gas.Sc,Y,In and Bi were selected as the internal standards to correct matrix effect.Linear relationships were found between signal intensities and mass concentrations of the 14 elements in definite ranges,with detection limits(3 s)in the range of 0.003-0.039μg·L~(-1).The method was used to analyze a CRM numbered GBW 10027,giving determination values of 14 elements in consistency with the certified values and RSDs(n=6)in the range of 1.6%-14%.
The sample(0.500 0 g)was digested with 3 mL of nitic acid and 2 mL of hydrogen peroxide,and Na,Mg,Ca,Al,Cu,Zn,Fe,Mn,Se,Pb,Cd,As,Hg,Cr in the sample solution were determined by ICP-MS.Acidity of φ 0.5% HNO_3 of the sample solution was adopted to enhance signal intensities of the 14 elements.The instrument was washed with 100μg·L~(-1) Au in φ 5% HNO_3 solution between 2 determinations to lower the adsorption effect of Hg.Mass spectral interference was eliminated using DRC mode with CH_4 as reaction gas.Sc,Y,In and Bi were selected as the internal standards to correct matrix effect.Linear relationships were found between signal intensities and mass concentrations of the 14 elements in definite ranges,with detection limits(3 s)in the range of 0.003-0.039μg·L~(-1).The method was used to analyze a CRM numbered GBW 10027,giving determination values of 14 elements in consistency with the certified values and RSDs(n=6)in the range of 1.6%-14%.
引文
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[7]李洁傲,赵月然,李军,等.电感耦合等离子体质谱法测定海参中17种金属元素的含量[J].理化检验-化学分册,2016,52(9):1108-1111.
[8]HU Z C,HU S H,GAO S,et al.Volatile organic solvent-induced signal enhancement in inductively coupled plasma-mass spectrometry:A case study of methanol and acetone[J].Spec Acta Part B,2004,59:1463-1470.
[9]GUO W,HU S H,WANG Y X,et al.Trace determination of selenium in biological samples by CH4-Ar mixed gas plasma DRC-ICP-MS[J].Micrchem J,2013,108:106-112.
[10]李冰,胡静宇,赵墨田.碰撞/反应池ICP-MS性能及应用进展[J].质谱学报,2010,31(1):1-11.
[11]邱静,韩芳,郑平,等.电感耦合等离子体质谱测定包装材料中8种可溶性元素[J].分析试验室,2011,30(10):20-23.
[12]刘宏伟,谢华林,聂西度.ICP-MS法测定苦杏仁中微量元素的研究[J].光谱学与光谱分析,2013,33(5):1354-1356.
[13]LI Y F,CHEN C Y,LI B,et al.Elimination efficiency of different reagents for the memory effect of mercury using ICP-MS[J].J Anal At Spectrom,2006,21(1):94-96.
[14]刘丽丽,王军,张丽娟.微波消解-同位素稀释质谱法测定鱼中汞含量[J].北京化工大学学报(自然科学版),2009,36(4):21-24.
[15]SCHAEFFER R,FRANCESCONI K A,KIENZL N,et al.Arsenic speciation in freshwater organisms from the river Danube in Hungary[J].Talanta,2006,69:856-865.
[16]胡圣虹,林守麟,刘勇胜,等.等离子体质谱法测定地质样品中痕量稀土元素的基体效应及多原子离子干扰的校正研究[J].高等学校化学学报,2000,21(3):368-372.