福建省地产茶叶中微量元素含量的分析

目的了解福建省不同地区不同品种茶叶中铁、锰、铜、锌、钴、硒、铬、镍等微量元素的含量分布,为茶叶种植、茶叶营养及卫生学提供科学依据。方法在福建省主要产茶地和市场随机抽取不同品种茶叶135份,用微波消解-电感耦合等离子体质谱法(ICP-MS)测定样品中微量元素含量。结果茶叶中8种微量元素含量组内变化趋势为锰铁锌铜镍铬钴≈硒,不同品种茶叶中8种微量元素的含量均不全相同,铁观音中锰元素含量最高,功夫红茶中铁、锌、铜和铬元素含量最高,白牡丹中镍元素含量最高,永春佛手中钴元素含量最高,正山小种中硒元素含量最高。闽北地区茶叶中铁、锌、铜、镍的平均含量高于闽南地区,差异均有统计学意义(P0.01),闽南地区的锰高于闽北地区,差异有统计学意义(P0.01),其他元素两地区相当(P0.05)。结论福建省地产茶叶中富含多种微量元素,且不同地区不同品种茶叶中各元素含量存在差异。     

微波消解-电感耦合等离子体质谱(ICP-MS)同时测定地沟油中微量元素

目的:测定地沟油中的微量元素含量。方法:采用HNO3-H2O2酸体系进行微波消解、电感耦合等离子体质谱法进行测定。结果:在优化的实验条件下,方法的检出限(3σ,n=11)为0.01~7.50μg/L;相对标准偏差为0.30%~14.92%;标准加入回收率为88.2%~111.3%。结论:元素Fe、Cr、Zn、Mn在地沟油中含量明显超出食用油,而Hg、Sn、Co、Sb、Tl、Mo无论在食用油还是在地沟油中含量均低于检测限。     

电感耦合等离子体-质谱法测定人尿中21种微量元素

目的 建立人尿中21种微量元素同时分析的电感耦合等离子体-质谱测定方法。方法 尿液经2%硝酸稀释10倍后,采用电感耦合等离子体（ICP）-四级杆质谱法（MS）检测。结果 采用内标法定量,各元素内标回归方程的决定系数均大于0.99,加标回收率在63.6%~101.5%之间。所测元素的相对标准偏差小于15%。各元素检出限在0.001μg/L~0.880μg/L之间。尿样内标元素45Sc的信号漂移在40%以内;74Ge,89Y和209Bi的信号漂移在30%以内;115In的信号漂移在20%以内。结论 ICP-MS方法简便、快速、灵敏、稳定,适合批量人尿中21种元素的分析。     

考核水样中19种微量元素的ICP-AES同时测定法

目的建立电感耦合等离子体-原子发射光谱法同时测定考核水样中铝、锑、砷、钡、铍、硼、镉、铬、铜、铁、铅、锰、钼、镍、硒、银、铊、钒、锌共19种微量元素含量的分析方法。方法优化了仪器条件,提高了信噪比,避免了谱线干扰,水样按考核要求用0.5%硝酸稀释后直接进样分析。结果 19种微量浓度在0～2.0μg/ml范围内呈良好线性关系,方法最低检出限在0.3～6.3μg/L,回收率为89.0%～105.1%,相对标准偏差(RSD)为0.18%～4.30%。结论该方法是一种快速,灵敏,准确的分析方法,可用于考核水样中19种微量元素的同时测定。     

ICP-MS法快速测定葡萄酒中11种微量元素

目的：探讨葡萄酒中11种微量元素的测定方法。方法：以Sc、Ge、Y作内标，采用电感耦合等离子质谱法（ICP-MS）分别测定了不同产地葡萄酒中Mg、Ca、Fe、Mn等11种微量元素的含量。样品用1％硝酸稀释后直接测定。结果：方法的线性范围宽，线性相关系数均〉0．999。测定试样中11种元素的相对标准偏差（n=7）均低于5．7％，各元素的加标回收率均在83．5％～104％。结论：方法操作简便、快速、灵敏、准确，不同产地的葡萄酒中均含有较丰富的微量元素。     

Content of macro- and microelements and evaluation of the intake of different dairy products consumed in Croatia

Macromineral and microelement contents were measured by inductively coupled plasma-optical emission spectrometry in 51 dairy products (milk, four types of cheese and butter). Significant differences in the concentrations of Ca, K, Na, Mg, Zn and Cu were observed (p < 0.05, all) between dairy products. Higher levels of Ca, Na, Mg and Se were measured in hard cheese than in semi-hard, fresh and cream cheese samples. The highest mean levels of elements were measured in products (mg kg⁻¹): milk: K 2070; hard fat cheese: Ca 10,700, Na 10,300, Mg 440, Zn 91.3, Se 0.78; cream cheese: Cu 3.12, Fe 3.9; butter: Se 0.79. The estimated daily intakes (EDIs) calculated for milk show contribution to the recommended dietary allowance (RDA) for the elements (%): Ca 42, K 13.2, Mg 10.3–13.3, Zn 11.4–15.7, Se 13.1. The highest contribution of elements to the RDA values was determined for hard fat cheese (%): Na 7.93, Zn 16.6–22.8, Se 28.4. However, a contribution to the RDA of less than 1% was determined for K, Mg and Fe in cheeses. The contribution of Cu to the RDA value ranged in cheese samples between 2.78 and 6.93%, though this was less than 1% in milk.     

Trace elements determination in edible seaweeds by an optimized and validated ICP-MS method

An optimized and validated inductively coupled plasma mass spectrometry (ICP-MS) method was used to analyze trace elements in seaweeds. Different volumes and rates of HNO₃ and H₂O₂, digestion times, and microwave power levels were tested to ascertain the best conditions for sample digestion. Analytical mass and instrumental parameters were selected to assure accurate and precise determination of As, Cd, Co, Cr, Mo, Ni, Pb, Sb, Se, and V by ICP-MS. The method was optimized and validated using biological Certified Reference Materials. In addition, some samples of seaweeds (Porphyra and Laminaria) from France, Spain, Korea, and Japan were analyzed using the optimized method. Porphyra presented higher concentrations of most elements, except for As, than Laminaria. Seaweeds from Korea and Japan tended to display the highest concentrations of Pb and Cd. In contrast, Spanish and French samples showed the highest levels of some micro-elements essential to human nutrition.     

Measurement of the total choline content in 48 commercial dairy products or dairy alternatives

In this work, the total choline and choline-containing moieties (free choline, glycerophosphocholine, phosphocholine, phosphatidylcholine, lysophosphatidylcholine and sphingomyelin) of 48 dairy products or dairy alternatives available in Canada were determined by hydrophilic interaction liquid chromatography-tandem mass spectrometry (LC–MS/MS). The average total choline content for one serving of fluid milk and alternative (i.e. 250 mL as defined by Canada's Food Guide) was 32.9 ± 2.4 mg for cow's milk, 24.9 ± 0.1 mg for goat's milk and 31.2 ± 4.2 mg for soy beverage. The average total choline content for one serving of yogurt (175 g) was 25.6 ± 3.2 mg. One serving of cheese (50 g) provided 7.1 ± 1.1 mg of total choline on average. Our data show that for dairy products there is a negative correlation between the total choline content on a dry weight basis and the fat content (r = −0.734, P < 0.001). Overall, we determined the choline content of a variety of dairy products which can supplement the data in the existing United States Department of Agriculture (USDA) choline database and be used in accurately estimating dietary choline intake in epidemiological studies. Hence, dairy products are a good source of choline with low fat products generally being a better source of choline than high fat dairy products.     

Essential and non-essential/toxic trace elements in whey protein supplements

Twenty-six (26) trace elements (essential and non-essential/toxic) were determined in 49 whey protein (WP) supplements available for sale in the Portuguese market by inductively coupled plasma – mass spectrometry. The most abundant essential trace element was Fe (13.7 ± 16.7 μg/g) and the least abundant was Co (0.040 ± 0.028 μg/g). The estimated daily intake was calculated and, considering a daily consumption of 50 g of WP supplement, on average, 100 % of the recommended dietary allowance for Mo and ca. 40 % for Se is met. A safety assessment was also performed based on the Permitted Daily Exposure limits settled by the USP, general chapter <2232> . The daily consumption of 50 g of WP supplement does not contribute for more than 12.1 % (Cd) of those limits, as regards As, Cd, Pb and Hg. Thus, WP supplements can be considered safe products, regarding the presence of potentially toxic elements.     

血清中21种元素的直接进样动态反应池电感耦合等离子体质谱测定法

目的 建立测定大批量血清样品中多种元素的检测方法.方法 血清样品用1％硝酸稀释3倍后,应用动态反应池电感耦合等离子体质谱仪(inductively coupled plasma mass spectrometry,ICP-MS)同时测定铍(Be)、铝(Al)、锰(Mn)、钒(V)、铬(Cr)、铁(Fe)、钴(Co)、镍(Ni)、铜(Cu)、锌(Zn)、砷(As)、硒(Se)、钼(Mo)、银(Ag)、镉(Cd)、锑(Sb)、钡(Ba)、铊(Tl)、铅(Pb)、钍(Th)、铀(U)共21种元素.结果 各元素的检出限为0.001～0.0711μg/L,线性相关系数r≥0.999,相对标准偏差＜5％,方法回收率为90％～ 114％.用Seronorm Trace Elements Serum L-1 LOT 0903106作标样质控,检测结果与标准值吻合.结论 该方法简化了前处理过程,具有操作简单、快速、灵敏、准确等优点,完全可以满足测定要求.     

电感耦合等离子体质谱法测定食品中铀及其同位素比值

目的:建立食品中铀及其同位素比值的分析方法。方法:食品经湿法消化后直接用ICP-MS进行分析。结果:总铀的测定的精密度优于1.5%、检出限小于0.02μg/kg,加标回收为94.8%～101%;235 U/238 U同位素比值测定的精密度优于0.8%,标准物质的分析结果和证书值一致。结论:可采用ICP-MS准确测定食品中的铀及其同位素比值,方法简便、快速、准确。     

微波消解-电感耦合等离子体质谱法测定小麦中的8种元素

目的利用微波消解-电感耦合等离子体质谱法测定小麦中Pb、Cd、As、Cr、Se、Ni、Al、Cu的含量。方法样品经过微波消解后,用ICP-MS法同时测定小麦中Pb、Cd、As、Cr、Se、Ni、Al、Cu的含量,以45 Sc、72Ge、103Rh、209Bi作为内标元素采用电感耦合等离子体质谱法测定,用标准曲线法进行定量。结果小麦中Pb、Cd、As、Cr、Se、Ni、Al、Cu的回收率在95.6%~106.8%,线性相关系数(r)≥0.9995,Pb、Cd、As、Cr、Se、Ni、Al、Cu的检出限分别为0.0049μg/L、0.0023μg/L、0.012μg/L、0.016μg/L、0.026μg/L、0.0099μg/L、0.0070μg/L、0.0027μg/L;生物成分分析标准物质(小麦)的各元素的测定结果均在标准值不确定度范围内;同时对3份小麦样品进行连续6次测定,各元素的相对标准偏差(RSD)≤5%。结论本法线性范围宽、抗干扰能力强、测定周期短,完全满足分析的要求,适用于日常样品的检测。     

微波消解-电感耦合等离子体串联质谱法测定野生食用菌中14种金属元素

目的 建立野生食用菌中14种金属元素（Ba、Cd、Co、Cr、Cu、Fe、Hg、Mn、Ni、Pb、Ti、Tl、V、Zn）的微波消解-电感耦合等离子体串联质谱（ICP - MS/MS）测定方法。方法 样品经HNO3 - H2O2微波消解,采用ICP - MS/MS对野生食用菌中14种金属元素进行同时测定。在MS/MS模式下,以氧气或氢气为反应气,利用质量转移或电荷转移消除多原子粒子的质谱干扰。利用标准曲线法定量。结果 方法线性范围在0～200 μg/L（Hg为 0.00～50.00 μg/L）,相关系数大于0.9995,检出限为0.46～45.03 ng/kg,加标回收率为84.3% ～110.0%。通过分析国家标准参考物质紫菜（GBW10023）和芹菜（GBW10048）中的多种元素含量以验证方法准确度和精密度,测定结果在参考值范围内,RSD均小于4.0%。结论 该方法具有简单快速、准确等优点,适用于食用菌中14种金属元素的同时测定。     

应用ICP-MS与AAS测定食品中铅、镉、铜方法研究及比较

目的:建立微波消解、电感耦合等离子体质谱法(ICP-MS)同时测定食品中微量元素的方法,并与国标法原子吸收分光光度法(AAS)进行了比较。方法:应用微波消解进行样品前处理,使用电感耦合等离子体质谱与原子吸收分光光度计分别测定三十余种食品中铅、镉、铜含量。结果:线性相关系数均大于三个9,方法的精密度均小于8.0%,国家标准物质:小麦粉(GBW08503b)、杨树叶(GBW08513)、贻贝(GBW08571)测定值均在标准值范围内,两种方法的测定值基本吻合。结论:ICP-MS法3种元素可同时分析,抗干扰强,但仪器成本高;AAS法每一元素需分别测定,测定周期较长,干扰较大,特别是高盐样品需稀释后测定,但仪器成本低,普及率高。     

Recognition of organic rice samples based on trace elements and support vector machines

A simple approach is proposed for the authentication of organic rice samples. The strategy combines levels of concentration of trace elements and a data mining technique known as support vector machine (SVM). Nineteen elements (As, B, Ba, Ca, Cd, Ce, Cr, Co, Cu, Fe, La, Mg, Mn, Mo, P, Pb, Rb, Se and Zn) were determined in organic (n = 17) and conventional (n = 33) rice samples by quadrupole inductively coupled plasma mass spectrometry (q-ICP-MS) and the variations found in their elemental composition resulted in profiles with useful information for classification purposes. With the proposed methodology, it was possible to predict the authenticity of organic rice samples with an accuracy of 98% when using the 19 original elements. An accuracy of 96% was found using only the elements Ca and Cd.     

Major and trace elements levels in multifloral and unifloral honeys in Croatia

Different honey types were collected in Croatia during 2010 and 2011: 7 multifloral orchard honeys, 7 multifloral meadow honeys, 19 black locust, 9 chestnut, 11 lime and 6 sage honeys. Elements were measured using graphite (As, Cu, Cd, Pb, Se) and flame atomic absorption spectrometer (Ca, Fe, K, Mg, Na, Zn) and by mercury analyser (Hg). Significant differences in Ca, Fe, K, Mg, Zn, As and Hg levels were observed between honey types. In chestnut honey were determined (K, Ca, Mg: mg kg⁻¹; Hg, Ad, Cd: μg kg⁻¹): the highest concentrations of K 2824.4, Ca 486.7, Mg 59.1 and Hg 2.52; the lowest of As 24.1 and Cd 2.52. Lime honey has been shown the highest content of Cu (20.6 mg kg⁻¹), Zn (6.78 mg kg⁻¹), Cd (2.14 μg kg⁻¹) and Pb (810.3 μg kg⁻¹). The lowest levels of following elements were determined in black locust honey (Fe, K, Mg: mg kg⁻¹; Hg: μg kg⁻¹): Fe 2.77, K 304.7, Mg 8.02 and Hg 0.82. Sage honey had the lowest Ca and Na content (173.9 and 31.8 mg kg⁻¹). Among the multifloral honeys, the following was determined (Fe, Na, Cu: mg kg⁻¹; As, Pb: μg kg⁻¹): orchard honey – highest of Fe 5.17 and As 276.1, lowest Pb 301; meadow honey – highest Na 36.1, lowest Cu 4.38. The average Ca, Cu and Pb levels found in multifloral honey types were much higher than those reported in other European countries. Calcium levels in lime, chestnut and black locust were higher than those from other countries.     

A Brazilian Total Diet Study: Evaluation of essential elements

Total Diet Study (TDS) has been adopted worldwide and is based on the evaluation of food samples representing a Market Basket, which shows dietary habits of a large-scale population. This TDS presents results of the element concentrations, daily dietary intakes and contributions to the total daily intake of essential elements, Na, K, Ca, Fe, Zn and Cr in 30 food groups of a Market Basket of São Paulo State, Brazil. The methodology for the first Brazilian TDS for the São Paulo State population and its respective Market Basket was developed. Food consumption data and information were obtained from the National Household Food Budget Survey, Pesquisa de Orçamentos Familiares (POF) 2002–2003 conducted by the Brazilian Institute for Geography and Statistics, which includes 5440 foods. The selection criteria to carry out the Market Basket were the foods consumed at more than 2 g/day/person, which represented 72% of the total weight of the foods for this population. Element concentrations were determined by instrumental neutron activation analysis and ranged in mg kg⁻¹ as follows: Na: 1.5–256,185; K: 0.51–532; Ca: 22–1827; Fe: 0.08–49; Zn: 0.030–98; and in μg kg⁻¹ Cr: 2.6–799. The dietary intakes contributed by the Market Basket were: 1928 mg/day⁻¹ Na; 861 mg/day⁻¹ K; 275 mg/day⁻¹ Ca; 5.70 mg/day⁻¹ Fe; 4.25 mg/day⁻¹ Zn and 20.7 μg/day⁻¹ Cr. The observed low levels are probably due to the fact that Market Basket represented 72% of the weight of the household consumed foods. The highest contributions to the total intake of the essential elements were: salts, 78.9% of Na; breads, 36.9% of Fe and 46.4% of Cr; cereals, 18.7% of Zn; and milk/cream, 58.7% of Ca and 23.6% of K.     

电感耦合等离子体质谱法测定铊中毒事件中铊含量

目的：用电感耦合等离子体质谱法测定铊中毒样品并考察其方法学。方法：优化仪器工作参数,用内标溶液校正基体效应干扰,用电感耦合等离子体质谱测定各样品铊含量。结果：本法的检出限为0.008μg/L,回收率96.8%~104.8%。经测定在尿样和餐具中检出高浓度铊。结论：用电感耦合等离子体质谱法测定铊中毒样品是一种灵敏快速、简便准确的方法。     

全血中16种元素的电感耦合等离子体质谱同时测定

目的 建立全血样品中多种元素同时测定的检测方法.方法 全血样品用体积分数为5％的硝酸脱蛋白沉淀后离心取上清液,应用动态反应池电感耦合等离子体质谱仪( ICP-MS)同时测定铍(Be)、铝(Al)、锰(Mn)、钒(V)、铬(Cr)、钴(Co)、镍(Ni)、砷(As)、钼(Mo)、银(Ag)、镉(Cd)、锑(sb)、钡(Ba)、铊(Tl)、铅(Pb)、铀(U)16种元素.结果 各元素的检出限为0.01～6.51 μg/L,线性相关系数r≥0.999,相对标准偏差＜5％,方法回收率为105％～115％.质控采用Seronorm Trace Elements whole Blood L2LDT 0503109和GBW09139g 、GBW09140g,检测结果与标准值吻合.结论 该方法具有操作简单,快速,灵敏、准确等优点,适用于全血样品中多种微量元素的同时测定.     

面制食品中铝的电感耦合等离子体质谱测定方法

[目的]建立检测面制食品中铝含量的电感耦合等离子体质谱测定方法。[方法]使用高纯硝酸-过氧化氢混合体系,结合快速、简便的微波密闭高压消解技术,建立了面制食品中铝的电感耦合等离子体质谱测定方法。[结果]使用本测定方法有证标准样品测定的平均值与标准值吻合良好,方法的最低检出限为0.04 ng/ml,最低定量下限为0.05 mg/kg,加标样品回收率范围为95.2%～104.4%。[结论]本测定方法提供了极宽的动态线性范围,极低的检测限,并且操作简便、快速、干扰小,非常适合用于面制食品中铝的测定。