啤酒中重金属检测方法的建立及应用研究

重金属的污染及限量已受到各国严控,检测技术也得到快速发展。文中利用ICP-MS建立了啤酒中13种重金属及类金属的检测方法,各项指标均能满足国标中关于各重金属限量的检测要求。对市售48种啤酒进行抽样检测,结果表明,啤酒中的重金属没有超标现象。     

Speciation of selenium in selenium-enriched seeds,buckwheat (<Emphasis Type="Italic">Fagopyrum esculentum</Emphasis> Moench) and quinoa (<Emphasis Type="Italic">Chenopodium quinoa</Emphasis> Willdenow)

Buckwheat (Fagopyrum esculentum Moench) and quinoa (Chenopodium quinoa Willdenow) are widely used as food ingredients. The nutritional characteristics of these plants, i.e., high contents of proteins and amino acids suggest that selenium (Se) is preserved as selenoamino acid derivatives, in particular, selenomethionine (SeMet) in proteins, similar to selenized yeast. Therefore, buckwheat and quinoa are expected to be a good nutritional source of Se. Selenized buckwheat and quinoa were cultivated on Se-fortified soil using sparingly soluble Se salts, such as barium selenate and barium selenite. Se concentration in the edible parts of these plants was determined, and Se extraction efficiency with enzyme or alkali was evaluated. In addition, the chemical species of Se in the low molecular weight fraction of these plants were determined by HPLC-ICP-MS. Total Se concentrations in the edible parts of selenized buckwheat and quinoa were 170.4 ± 2.9 μg/g and 102.7 ± 2.4 μg/g wet weight, respectively. Thus, these selenized seeds were found to be Se accumulators. The results indicate that Se in selenized buckwheat exists mainly as SeMet, while Se in selenized quinoa exists not only as SeMet but also as selenate (Se(VI)) and non-protein forms.     

电感耦合等离子体质谱法(ICP-MS)测定甜菜颗粒粕中的砷含量

利用微波消化－电感耦合等离子体质谱法（ＩＣＰ－ＭＳ）测定甜菜颗粒粕中砷含量。对添加０．５,２．０,４．０ｍｇ／ｋｇ砷的甜菜颗粒粕样品,回收率为６８．２％－７１．４％。变异系数（ＣＶ）为２．７％。方法检测低限为０．１μｇ／ｋｇ。本方法具有前处理简单、快速,检测限低等特点,可用于甜菜粕中砷的检测和监控。     

湿法消解-电感耦合等离子体质谱法同时测定水生蔬菜中5种元素

目的　建立湿法消解/电感耦合等离子体质谱法（inductively coupled plasma mass spectrometry, ICP-MS）测定8种水生蔬菜中5种元素的方法。方法　样品在混合酸（硝酸+高氯酸=4+1, V/V）介质中消解,消解后,将消化液用水转移至25 mL容量瓶,并用ICP-MS同时测定水生蔬菜中总As、Cd、Cr、Ni和Pb这5种元素的含量。结果　5种元素的标准曲线线性范围可达0μg/L~200μg/L,相关系数：0.9992~0.9998,检出限：0.009 μg/L~0.025μg/L,定量限：0.030μg/L~0.083μg/L,回收率：89.4%~112.6%,RSD(n=11)：1.20%~1.86%。80份水生蔬菜样品中5种元素的含量均低于国家标准规定的食品中污染物限量。水生蔬菜不同种类间,5种元素的含量有显著差异。结论　湿法消解/ICP-MS方法直观、快速、准确、可靠,适于水生蔬菜中多元素同时测定。     

炭黑氨基柱净化HPLC-ICP-MS测定黄酒中砷形态及含量

建立了一种同时测定黄酒中亚砷酸根、砷酸根、砷甜菜碱、一甲基砷酸和二甲基砷酸等5种砷形态的高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)分析方法。黄酒经炭黑氨基柱净化,体积分数为10%甲醇水溶液洗脱,采用Hamilton PRP-XIO0阴离子交换色谱柱(4.1 mm×250 mm,10 μm),60 mmol/L硝酸铵梯度洗脱,高效液相色谱分离,电感耦合等离子体质谱进行定性和定量分析。在0.5～20.0 μg/L范围内各砷形态线性良好,相关系数R均＞0.999;加标回收率85%～92%,相对标准偏差(RSD)1.4%～5.2%;5种砷形态的定量限均为0.10 μg/L,检出限均为0.03 μg/L。利用该方法对不同年份、不同企业及不同类型的黄酒进行了检测,该方法适用于黄酒中砷残留的分析检测。     

Quantification of trace elements in raw cow’s milk by inductively coupled plasma mass spectrometry (ICP-MS)

The levels of trace elements are an important component of safety and quality of milk. While certain elements such as chromium are essential at low levels, an excess can result in deleterious effects on human health. International quality control standards for milk are published by the Codex Alimentarious Commission and levels of heavy metals in milk intended for human consumption are routinely monitored. This paper describes a new method for demonstrating the levels of V, Cr, Mn, Sr, Cd and Pb in raw cow’s milk, using an ICP-MS. Samples (n = 24) of raw cow’s milk were collected from dairy farms close to mines in Gauteng and North West Provinces of South Africa. In order to destroy organic matrix, each freeze dried milk sample was mineralised by using a microwave assisted digestion procedure. Concentrations of trace elements in digested milk samples were measured by ICP-MS. A whole milk powder reference material (NIST SRM 8435) was used to evaluate the accuracy of the proposed method. It was found that the levels of V, Cr, Mn, Sr, Cd and Pb obtained using the new method showed concordance with certified values.     

ICP-MS法同时测定地表水中21种痕量元素

以6 Li、Sc、Ge、Y、In、Bi 6种元素作内标校正系统,采用电感耦合等离子体质谱法(ICP-MS)同时测定地表水中的Be、Mg、Ca、V、Cr、Mn、Co、Ni、Cu、Zn、As、Se、Mo、Ag、Cd、Sb、Bs、Tl、Pb、Th、U 21种痕量元素,结果表明:各元素的线性系数均>0.999 5,方法检出限为0.006～0.738μg/L,标准样品的测定值均在标准范围内且RSD<4.22%,样品中各元素的加标回收率为95.0%～116.1%。     

碲化镉溶液中无机痕量杂质成分分析标准物质研制

本文研制了2 mg/g碲化镉(CdTe)溶液中无机痕量杂质成分分析的5种标准物质,每种包含21种杂质元素,浓度分别为0、1、2、4、8 ng/g。通过辉光放电质谱(GD-MS)法对CdTe原料纯度进行测量,筛选得到纯度>99.999%的高纯原料;使用HCl-HNO₃混酸将其溶解,再根据成分设计定量添加杂质元素,制备得到标准物质候选物。建立了基体匹配-内标校正-电感耦合等离子体质谱法用于标准物质定值与均匀性、稳定性检验,采用标准物质EB507验证方法可靠性。对包装容器溶出进行考察,以高密度聚乙烯(HDPE)作为包装容器可满足要求。采用建立的方法对全部元素进行检验,结果表明,标准物质均匀性以及长、短期稳定性良好,有效期12个月。通过8家实验室联合定值的方式,对标准物质中21种元素进行定值,以算数平均值作为标准值,并对不确定度进行全面、系统地评估。该系列基体标准物质填补了国内外空白,对于验证测量方法的可靠性、确保测量结果的一致性与溯源性具有重要作用。     

锍锑试金-电感耦合等离子体质谱法测定矿石中铂族元素

在锍试金配料中加入0.2 g锑粉进行熔炼,由于锑的保护作用,试金扣经水浸泡粉化后用(1+1)盐酸分解时锇不损失。铂族硫化物滤渣加10 mg锑粉保护,用2 mL王水在240℃下密闭消解1.5 h可完全溶解,试液采用ICP-MS测定。方法对铂族元素(钌、铑、钯、锇、铱和铂)检出限在0.03~0.16 ng/g之间,相对标准偏差(RSD,n=6)为3.9%~8.9%,国家标准物质测定值和认定值基本吻合,方法还可实现氧化镍源的提纯和循环使用。     

铅染毒大鼠血液中铅与其他元素含量的相关性研究

研究了铅染毒大鼠血液中铅与其他元素之间的关系。选取75只健康的4周龄雄性Sprague Dawley大鼠(SD大鼠),随机分为25组,各组染毒剂量均不相同。在实验开始的第40、80、120天,分别从各组中随机选取1只大鼠,乙醚麻醉后取股动脉血。用电感耦合等离子体质谱（ICP-MS）法测定血中的24种元素含量,并对铅与其他元素做相关分析。研究发现：在不同染毒周期,染毒剂量与血铅浓度的关系各有不同。血铅浓度随染毒时间的延长而升高,但染毒剂量在5~70 mg•kg^-1时,80天染毒组的血铅浓度反而高于120天染毒组;血铅与其他元素含量的相关性随染毒周期的变化而变化。