微波消解-ICP-MS同时测定大米中铅·镉和砷

[目的]建立微波消解-ICP-MS同时测定大米中铅、镉、砷的分析方法。[方法]将供试大米样品加入硝酸,经微波消解处理后,用电感耦合等离子质谱仪(ICP-MS)同时分析消解液中铅、镉、砷的含量。[结果]在试验优化条件下,该方法对铅、镉、砷的检出限分别为0.30、0.01、0.06μg/L,选用的国家标准物质的测定值在标准参考值范围内,相对标准偏差在6.0%以内。[结论]该方法简便高效,准确度高,精密度好,适用于大米等农产品中重金属元素铅、镉、砷的分析。     

碰撞反应池-电感耦合等离子体质谱法测定市售鱼丸中硼含量

[目的]建立密闭高压消解-电感耦合等离子体质谱法分析鱼丸中总硼含量的方法。[方法]鱼丸样品经HNO3-H2 O2处理后,以45 Sc为内标元素消除非质谱干扰,以氦气为碰撞反应气消除质谱干扰,用电感耦合等离子体质谱仪直接测定硼含量。[结果]在优化的试验条件下,方法的检出限为0.33μg/L,标准曲线的回归系数为0.9998。在高、中、低3个添加水平下,样品的回收率为96.8%~114.1%,相对标准偏差为4.6%~6.2%。选用3种国家有证标准物质进行测定,测定值与参考值一致,结果满意。[结论]该试验方法具有准确、快速、检出限低及线性范围宽等优点,适用于鱼丸中硼含量的检测。     

Discrimination of geographical origin of rice (Oryza sativa L.) by multielement analysis using inductively coupled plasma atomic emission spectroscopy and multivariate analysis

This study aims to determine the authenticity of the geographical origin of rice using inductively coupled plasma atomic emission spectroscopy (ICP-AES) and chemometrics. The profiles of 25 elements in brown rice measured by ICP-AES were subjected to data-mining processes, including principal component analysis (PCA) and partial least-squares discriminant analysis (PLS-DA). PLS-DA clearly discriminated the geographical origin of rice samples grown in three countries. Eleven elements (Cu, Ag, Zn, Cr, Ca, Ba, Cd, Bi, K, Pb, and In) significantly contributed to the ability to discriminate the geographical origin of the rice. These results demonstrate the use of multielement profiling combined with chemometrics as a tool for discriminating food origins. This study extends our knowledge about the applications of both multielement profiling and chemometrics for the determination of food authenticity, and thus can be useful for controlling the geographical origin of rice by governmental administration and protecting consumers from improper domestic labeling.     

ICP-MS法测定沙棘维生素P粉中13种微量元素含量

沙棘维生素P粉样品经微波消解处理,采用电感耦合等离子体质谱法测定样品中铁、硒、锌、钾、钠、钙、镁、铜、锰、铅、砷、汞、镉等13种微量元素的含量。使用动态反应池技术消除了多原子离子对部分被测元素的干扰。方法快速准确、灵敏度高,加标回收率在95.2%～101.8%之间,相对标准偏差小于3.0%。     

电感耦合等离子体质谱法(ICP-MS)测定碳酸饮料中的5种重金属元素

建立一种超声处理、电感耦合等离子体质谱法同时测定碳酸饮料中铬、砷、镉、汞、铅的方法。该方法检出限为0.001～0.007μg/L,加标回收率为86.5%～106.1%,变异系数(RSD,n=6)为0.76%～8.41%,测定结果满足分析要求。     

Losses of essential mineral nutrients by polishing of rice differ among genotypes due to contrasting grain hardness and mineral distribution

The effect of different polishing techniques on loss of mineral elements from rice grains was quantified using a panel of indica and tropical japonica genotypes, previously classified as differing in ease of polishing. Gradients in mineral elements across the bran-endosperm interface were quantified using micro-scaled precision abrasive polishing in combination with inductively coupled plasma mass spectrometry and synchrotron X-ray fluorescence microscopy. Frictional polishing, similar to that of commercial mills, i.e. 8–10% loss of grain weight, reduced the concentration of Fe, Mg, P, K and Mn by 60–80% in all genotypes. Following gentler polishing (3–5% weight loss), genotypes classified as difficult to polish showed smaller decreases in Fe, Mg, P, K and Mn compared to genotypes classified as easy to polish. The concentration of other elements, e.g. Zn, S, Ca, Cu, Mo and Cd, showed comparable reductions (<30%) irrespective of polishing technique or ease of polishing. The different patterns of polishing losses of minerals reflected their distribution within the grain. Five-fold differences in the reduction of Zn concentration during polishing were observed for different genotypes which started with similar Zn concentrations in the unpolished grain, thus showing clear potential for selecting genotypes with reduced polishing losses of Zn.     

微波消解-ICP-MS测定剑麻叶中微量元素钼

采用微波消解方法处理剑麻叶片样品,以铟(115In)为内标元素进行校正,优化ICP-MS仪器工作参数等技术,测定剑麻叶片中微量元素钼的含量。结果表明：钼的检出限为0.025 μg/L,回收率为96%～104%,相对标准偏差(RSD)为0.87%,同时测定国家标准物质菠菜(GBW10015)中的钼,分析结果在标准值范围内,显示微波消解-ICP-MS方法具有检出限低、快速、简便、准确等特点。     

薯莨块茎中氨基酸及矿质元素成分分析

[目的]分析测定薯莨（Dioscorea cirrhosae Lour.）块茎中的氨基酸和矿质元素的种类及含量,评价薯莨的营养价值,为薯莨的开发利用提供理论依据。[方法]采用高效液相色谱法测定氨基酸含量;采用电感耦合等离子质谱法测定矿质元素含量。[结果]测得氨基酸16种,必需氨基酸占氨基酸总量的37.98%,其中天冬氨酸、谷氨酸、亮氨酸含量较高,居于前3位,蛋氨酸含量最低;薯莨块茎中富含K、Ca、Na、P和Mg 5种常量元素和B、Mn、Mo、Co、N、iCr、Cu、Se、Fe、Sr、Zn、Ba、Cd和Li14种微量元素。[结论]测得署莨块茎中富含多种营养成分及药效成分,该研究为薯莨的开发利用提供了理论依据。     

烹饪火锅用容器重金属溶出比较研究

运用微波消解预处理纯水和酸菜,用HG-AFS、ICP-MS法测定紫铜、不锈钢和陶瓷容器分别熬煮纯水、酸菜的过程中,其汤料、酸菜样品中砷、汞、铅、镉、铬、镍等的含量变化.结果表明:在紫铜、不锈钢和陶瓷容器中熬煮纯水6 h时,均无砷、汞、铅、镉、铬、镍溶出.但长时间熬煮酸菜,紫铜锅体有较多汞、铅和少量镉、镍、铬溶出;不锈钢制锅体有较多铅、铬、镍和少量镉溶出;陶瓷制锅体有一定量的汞与微量铅、镉溶出.说明食用酸菜类火锅时,宜用陶瓷容器并将时间控制在2 h内.     

电感耦合等离子体质谱法测定土壤中的总碘

采用碱液热浸提法处理土壤样品,通过电感耦合等离子体质谱法(ICP-MS)测定土壤中碘元素的总量。对前处理的3大参数——碱度、温度和时间进行试验摸索,得出适用于土壤的最佳浸提条件。测定结果显示,该方法的线性范围为0~500μg/L,线性相关系数0.999 8,方法检出限0.12μg/g,加标回收率为91.0%~104%,RSD均小于5%。综上,该法是一种能够快速、灵敏、准确地测定土壤样品中碘元素的先进方法。