微波消解ICP-OES测定牛蒡茶中的矿质元素

采用HNO3/H2O2微波消解的制样方法,利用全谱直读电感耦合等离子原子发射光谱仪（ICP-OES）对牛蒡茶中的Al、As、Ba、Ca、Cd、Cr、Cu、Fe、K、Mg、Mn、Na、Ni、P、Pb、Sr、Ti、Zn等18种矿质元素进行了测定。结果表明,牛蒡茶中含有人体必需常量元素K、Na、Ca、Mg、P和人体必需微量元素Cu、Fe、Mn、Ni、Ti、Zn,以及人体非必需的微量元素Al、Ba、Sr,而有害元素As、Pb、Cr、Cd均未检出。并建立了一种牛蒡茶中矿质元素的分析测试方法,各元素的回收率均在93.7%¹07%,相对标准偏差在1.31%².31%,检出限低且满足各元素分析要求,此方法具有简捷、快速、准确的特点。      

MINERAL COMPOSITION OF MEDLAR (MESPILUS GERMANICA) FRUIT AT DIFFERENT STAGES OF MATURITY

Abstract The mineral composition of medlar fruit collected (June 15 - October 8) in Turkey at five stages of development was studied. In the fruit, 32 minerals were analyzed and 16 minerals (Al, Ba, Ca, Cu, Co, Fe, K, Li, Mg, Mn, Na, Ni, P, Sr, Ti and Zn) were present at detectable levels. The ripe medlar fruit was richest in potassium (7370 μg/g dry wt), calcium (1780 μg/g dry wt), phosphorus (1080 μg/g dry wt), magnesium (661 μg/g dry wt) and sodium (183 μg/g dry wt). During the fruit development, Al, Ba, Fe, Mn, P, Sr, and Zn were highest in August (unripe fruits) while the concentrations of K, Ca, Mg and Cu gradually decreased throughout development. The ripe medlar fruit is an important source of nutritionally needed minerals and trace elements, in particular Ca, Cu, Fe, K, Mg, Mn, Na and Zn, for human populations in southeastern Europe, Turkey and Iran.     

电感耦合等离子体原子发射光谱法同时测定江西脐橙中多种微量元素

采用硝酸-高氯酸对江西赣南8个县所产的脐橙样品进行消解,电感耦合等离子体原子发射光谱法(ICP-AES)同时测定试样中Al、As、Ba、B、Ca、Co、Cr、Cu、Fe、K、Li、Mg、Mn、Ni、P、Pb、Zn、Be、Cd、Se、Sr、La、Ce、Y、Sm、Lu等元素的含量。该法的相对标准偏差为0.42%～4.51%,加标回收率为87.7%～114.1%。实验结果表明:脐橙中含有丰富的K、Ca、P和Mg,不同县所产的脐橙各种微量元素含量存在一定差异。     

Contribution to the study of avocado honeys by their mineral contents using inductively coupled plasma optical emission spectrometry

Avocado honey samples were analyzed by inductively coupled plasma optical emission spectrometric. First, the botanical origin of the honeys was confirmed by melissopalynological analysis. Twenty-four minerals were quantified for each honey sample. The elements Al, Ba, Ca, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, P, Pb, S, Se, Si and Zn were detected in all samples; seven elements were very abundant (Ca, K, Mg, Na, P, S and Si), six were not abundant (Al, Cu, Fe, Li and Zn) and 11 were trace elements (As, Ba, Cd, Co, Cr, Mo, Ni, Mo, Pb, Se, Sr and V).     

Investigation of major and trace elements and their distributions between lipid and non-lipid fractions in Brazil nuts by inductively coupled plasma atomic optical spectrometry

Major (Ca, Mg, P) and trace (As, Al, Ba, Cd, Cr, Cu, Fe, Hg, Mn, Ni, Se, Zn) elements were determined in Brazil nuts by means of inductively coupled plasma atomic optical spectrometry (ICP-OES) and five of them were measured for the first time. For measurement of As, Hg and Se levels, hydride generation was used as the sample treatment method. The element concentrations were compared with recommended dietary allowances and upper tolerable levels. The distributions of the elements between lipid and lipid-free fractions were investigated with the use of solvent extraction. Two extractants (petroleum ether and chloroform:methanol 2:1) were applied. Most of the Cr, Fe and Ni contents were found in the lipid fraction, while Ba, Ca, Cu, Mn, P and Zn were mainly bonded with defatted nut residue. Al, Mg, Se, Sr were only present in the defatted fraction.     

绿豆中矿质元素组成的测定与分析

经HNO3/H2O2湿法微波消解制样,利用全谱直读电感耦合等离子原子发射光谱法（ICP-OES）,全面详细地分析测定了陕北地区产绿豆中的矿质元素。测定结果显示,绿豆中含有K、P、Mg、Ca、Si、Fe、Al、Na、Zn、B、Mn、Cu、Sr、V、Ba等15种矿质元素。测定结果相对标准偏差RSD值在0.48%～5.38%之间,分析方法回收率在91.9%～108.4%之间。测定方法可以多元素同时测定,且快速、简单、可靠,能满足实际样品分析要求,分析结果可为绿豆的相关研究提供参考。      

Minor and trace elements in different honey types produced in Siena County (Italy)

The concentrations of 23 chemical elements (Al, As, Ba, Ca, Cd, Co, Cr, Cu, Fe, Hg, K, Mg, Mn, Na, Ni, Pb, Sb, Se, Sr, Th, Tl, U, Zn) were determined in 51 honey samples of different botanical origin produced in Siena County (Italy). K, Ca, Na and Mg were the most abundant elements, with mean contents of 1195, 257, 96.6 and 56.7 mg/kg, respectively. The Fe, Zn and Sr contents generally ranged from 1 to 5 mg/kg. Except for Ba, Cu, Mn and Ni, the trace element contents were below 100 μg/kg. The analytical data indicated a good level of quality of the honeys, especially with regard to the concentrations of toxic trace elements, such as As, Cd, Pb and Sb, and suggested a significant influence of the botanical origin on the element composition. Some local geological and geochemical features also seemed to affect the chemistry of the honey.     

Concentrations and bioconcentration factors of minerals in yellow-cracking bolete (xerocomus subtomentosus) mushroom collected in noteć forest, poland

Abstract: Yellow‐cracking Bolete (Xerocomus subtomentosus) mushrooms and soil were collected from Note? Forest–a large forested enclave in western part of Poland. Mercury was determined by cold vapour atomic absorption spectroscopy and the other elements by inductively coupled plasma atomic emission spectroscopy. K, P, and Mg were particularly abundant, with mean values of 46000, 8400, and 1100 mg/kg dry weight (dw) in caps followed by Na, Rb, Zn, and Ca with mean concentrations of 580, 350, 200, and 170 mg/kg dw, respectively. In descending order, the mean concentrations of Fe, Al, Cu, and Mn were 52, 49, 46, and 14 mg/kg dw, while the mean for the remaining elements was around 1.0 mg/kg dw or less. The elements such as Ca, Cu, Hg, K, Mg, Na, P, Rb, Zn, Ag, Cd, and Ni were accumulated (with bioconcentration factor (BCF) > 1), while Al, Ba, Fe, Mn, Sr, Co, Cr, and Pb were excluded (BCF < 1) in the fruiting bodies. The Pb and Cd content did not exceed the maximum levels set by the EU for cultivated mushrooms. Mercury in a conventional meal (300 g) portion of Yellow‐cracking Bolete was far below the provisionally tolerable weekly intake of 0.004 mg/kg body weight (bw) as reevaluated recently by WHO. Practical Application: The method presented in this study allows one to determine the content of 20 elements (Ag, Al, Ba, Ca, Cd, Co, Cr, Cu, Fe, Hg, K, Mg, Mn, Na, Ni, P, Pb, Rb, Sr, and Zn) in caps and stipes of Yellow‐cracking Bolete (Xerocomus subtomentosus) mushrooms and soil samples collected from Poland. This study has revealed that the total Cd, Hg, and Pb dose provided to human body due to consumption of Yellow‐cracking Bolete does not pose threat to a consumer's health.     

不同麦类麸中无机元素的含量分析

建立电感耦合等离子体发射光谱(inductively coupled plasma-optical emission spectrometry,ICP-OES)法测定荞麦麸皮、燕麦麸皮和黑麦麸皮中14种无机元素的分析方法。选择硝酸+过氧化氢为消解溶剂,麦类麸皮经微波密闭消解后直接分析。通过优化ICP-OES工作条件以及选择待测元素分析波长,确保仪器处于最佳工作状态,研究共存元素的光谱干扰及其消除。方法的检出限在0.26~52.66μg/L范围内;各元素的线性相关系数在0.999 5~0.999 9之间;通过测定国家标准物质小麦(GBW10011),表明方法具有良好的准确性和较高的精密度。     

Mineral profile of “fino” wines using inductively coupled plasma optical emission spectrometry methods

Fifty wines from the Denomination of origin (DO) of Condado de Huelva were analysed for mineral content by measuring 12 elements (Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, P, Sr and Zn) using Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). Samples were previously digested by heating with H₂O₂/HNO₃ mixture. The results obtained showed that metal data set were non-normally distributed and accordingly, non-parametric statistics were applied. The average levels (medians) of these elements found in the samples are as follows, in mg/L: 2.54 (Al); 0.06 (Ba); 82.58 (Ca); 0.21 (Cu); 3.53 (Fe); 865.34 (K); 68.87 (Mg); 0.71 (Mn); 32.77 (Na); 71.61 (P); 0.48 (Sr); 0.56 (Zn). The interrelation of metal couples was studied through the Spearman non-parametric sample correlation, being Fe/Al, P/Mg, and Zn/Ba the most important correlations established. As a result of this study, we can suggest that the contribution to the safety intake limits (per week) of the studied elements through the wine consumption is not significant. Actually, they range between 0.1% in Fe and 11.9% in Mg, for normal drinkers.     

大连湾牡蛎中微量元素的分析

采用火焰原子吸收光谱法(FAAS)对牡蛎及其内脏中钠、铜、锌、铁、铅、锶、锰、钙8种微量元素的含量进行连续测定,并时其测定结果作对比分析.同时考察不同消解方法对分析结果的影响,并用加标回收法对比检验方法的可靠性.结果表明:微渡消解法效果较好,相对标准偏差在3.04%以下,回收率为96.89%～104.33%之间.牡蛎中含有丰富的微量元素Na、Cu、Zn、Fe、Sr、Mn、Ca,特别是Cu、Zn含量较高.牡蛎内脏中Na、Cu、Zn、Fe、Mn含量高于完整牡蛎中含量,Sr、Ca含量低于完整牡蛎中含量.牡蛎及其内脏中均未检出Pb.     

原子吸收光谱法测定辣椒及辣椒食品中的微量元素

应用火焰原子吸收光谱法对辣椒及辣椒食品中的Cu、Na、Fe、K、Sr、Mg、Ca、Mn、Zn等9种微量元素的含量进行测定分析。结果显示:Cu、Na、Fe、K、Sr、Mg、Ca、Mn、Zn的标准曲线相关系数为0.9999、0.9820、0.9997、0.9927、0.9982、0.9965、0.9991、1.0000和0.9985;辣椒及辣椒食品中均能检出这9种微量元素,其中辣椒籽中的Cu、Mg、Mn、Zn含量很高;制成辣椒食品后,Na含量大幅度增加,而相对于其他香辣酱,鲜食辣椒酱Na含量最低;辣椒制成辣椒食品后部分微量元素富集(如Cu、Na、Fe、Ca等)比鲜冻辣椒中微量元素含量高。      

电感耦合等离子体质谱法(ICP-MS)测定砂糖中31种微量元素

利用微波消化－电感耦合等离子体质谱法（ＩＣＰ－ＭＳ）同时测定了白砂糖和赤砂糖中３１种微量元素。白砂糖中检测出２３种,赤砂糖中检出２７种。结果表明,Ｃａ,Ｍｇ,Ｋ,Ｆｅ,Ｍｎ,Ｃｕ等６种元素在赤砂糖中含量比在白砂糖中含量高出４￣４００倍。Ｌｉ,Ｂａ,Ｎａ,Ｐ,Ａｌ,Ｖ,Ｃｒ,Ｎｉ,Ｚｎ,Ｇａ,Ｓｒ,Ａｇ,Ｓｎ,Ｓｈ,Ｂａ,Ｈｇ,Ｐｂ等１７种元素在白砂糖和赤砂糖中的含量无显著差别。本方法具有前处理简单     

ICP-OES法分析测定大红袍花椒中的矿质元素

经湿法微波消解制样,利用全谱直读电感耦合等离子发射光谱法(ICP-OES)对大红袍花椒中的矿质元素进行全面详细的分析测定。测定结果表明,花椒中含有K、Ca、P、Mg、S、Al、Fe、Sr、Na、Mn、B、Zn、Ba、Cu、Ti、Cr等16种矿质元素,常量矿质元素中钾和钙的含量较高,微量元素中,铝、铁、锶、锰、硼含量丰富。分析方法回收率在90.1%～109.1%之间,测定结果相对标准偏差在0.55%～8.95%之间。该方法简单、快速、可靠、灵敏度高,且多元素可同时测定,能满足实际样品分析要求。分析结果可为花椒的相关研究提供参考。     

Simplified multi-element analysis of ground and instant coffees by ICP-OES and FAAS

A simplified alternative to the wet digestion sample preparation procedure for roasted ground and instant coffees has been developed and validated for the determination of different elements by inductively coupled plasma optical emission spectrometry (ICP-OES) (Al, Ba, Cd, Co, Cr, Cu, Mn, Ni, Pb, Sr, Zn) and flame atomic absorption spectrometry (FAAS) (Ca, Fe, K, Mg, Na). The proposed procedure, i.e. the ultrasound-assisted solubilisation in aqua regia, is quite fast and simple, requires minimal use of reagents, and demonstrated good analytical performance, i.e. accuracy from ?4.7% to 1.9%, precision within 0.5–8.6% and recovery in the range 93.5–103%. Detection limits of elements were from 0.086 ng ml^?1 (Sr) to 40 ng ml^?1 (Fe). A preliminary classification of 18 samples of ground and instant coffees was successfully made based on concentrations of selected elements and using principal component analysis and hierarchic cluster analysis.     

Multi-element analysis of tea beverages by inductively coupled plasma atomic emission spectrometry

The metal content of several tea beverages, infusions, instant and tea soft drinks was determined. Eleven metals Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Sr and Zn were determined by inductively coupled plasma atomic emission spectrometry (ICP–AES). A study of the differences in the metal contents of tea beverages has been carried out. Pattern recognition techniques such as principal components analysis and linear discriminant analysis were used to discriminate between the tea beverages. The metal intake related to tea consumption has also been studied.     

百香果中矿物元素分析

采用高压密封硝化罐消解样品,应用ICP-AES 法测定百香果果汁、果皮、种仁中20 种矿物元素 (Na、K 、C a 、Mg、Z n 、F e 、S r 、Cu 、Co 、Mn、Ge 、S e 、S n 、B a 、A l 、P b 、Hg、As 、C r 、Cd) 的含量,设计正交试验方案,通过方差分析选择最佳的试验操作条件,其回收率在95.0%～104.0% 之间,相对标准偏差小于2.15%。实验结果表明：百香果果汁、果皮、种仁中均含有丰富的Na、K、Ca、Mg、Zn、Fe、Ge等对人体有益的矿物元素,而对人体有害的元素均未检出,营养价值高,极具开发价值。     

Mineral Composition of Fresh and Cured Jellyfish

The inorganic constituents of fresh and cured jellyfish (Rhopilema esculentum), including Zn, Co, Ni, Ba, Mn, Fe, Mg, Ca, Cu, Al, Sr, Mo, Cr, Cd, Pb, Si, V, Ti, Na, K, Li, and Rb, were determined by using inductively coupled plasma optical emission spectrometry. The fresh and cured jellyfish were treated by lyophilization and microwave digestion in turn. Zn, Co, Fe, Mg, Ca, Al, Sr, Cr, Li, and K were used as the added standards to evaluate accuracy. The results show that different parts of jellyfish, such as the umbrella, oral arms, and gonads, contain different amounts of inorganic elements. The relative standard deviation values (RSD) of all elements range from 0.8% to 8.6%. For most of determined elements, RSD values are under 5%. All inorganic elements of the jellyfish can be determined simultaneously after once dissolution. The method is accurate, rapid, and convenient to determine inorganic constituents of the biological sample containing high water content.     

绿豆、红小豆和黑豆种皮18 种元素分析

为全面了解绿豆皮、红小豆皮和黑豆皮的18 种元素含量,充分开发利用豆皮资源,提高豆类加工产品
的附加值,用元素分析（elemental analyzer,EA）仪和电感耦合等离子体发射光谱（inductively coupled plasmaatomic
emission spectrometer,ICP-AES）仪测定了3 种豆皮的N、C、S、Ca、Mg、K、P、Na、B、Ba、Co、
Cr、Cu、Fe、Mn、Ni、Zn和Sr元素含量。结果表明,EA仪测定豆皮中N、C和S方法检出限为32～96 μg/g,回收
率为97%～115%,相对标准偏差为0.20%～2.63%（n=5）;ICP-AES测定豆皮中Ca、Mg、K、P、Na、B、Ba、
Co、Cr、Cu、Fe、Mn、Ni、Zn和Sr元素方法检出限为0.02～152 μg/g,回收率为84%～118%,相对标准偏差为
0.44%～4.46%（n=5）。黄豆标准物N、Mg、P、B、Ba、Co、Cr、Mn、Ni、Zn和Sr元素测定值在推荐范围内,
S、Ca、K、Na、Cu和Fe元素测定值接近推荐值。分析方法快速、简便,达到了应用的要求。     

加工精度对大米矿物元素指纹信息影响研究

矿物元素指纹分析技术已逐渐被应用到农产品的产地溯源中,大米中的矿质元素指纹信息的稳定性不仅与环境(地域和年际)密切相关,还受品种和加工精度的影响。研究农产品矿物元素指纹信息在不同加工等级与不同品种间的稳定性,解析品种、加工精度及其交互作用对各元素含量变异的贡献率,筛选出受品种、加工精度影响较小的元素作为产地溯源的指纹信息。可为农产品产地矿物元素指纹溯源技术的应用提供理论参考。本研究以水稻作为模式生物,于2013年收获期在黑龙江同一地市的3个品种的水稻样品,加工成5个不同等级,利用电感耦合等离子体质谱仪(ICP-MS)测定不同等级大米中49种矿物元素的含量。对数据进行单因素方差分析、多因素方差分析。大米中元素Na、Mg、Al、K、Ca、Cr、Mn、Fe、Co、Cu、Zn、Rb、Sr和Ba含量与加工精度密切相关;元素Na、Mg、Al、K、Ca、Cr、Mn、Cu、Zn、Rb和Mo含量与品种密切相关;在今后产地溯源技术筛选溯源指标时应考虑这些元素。