电感耦合等离子体质谱法测食品中的铅、镉、砷、汞

电感耦合等离子体质谱（ICP—MS）法相比于传统的化学法及原子吸收法具有以下优点：测定金属元素可一次进样同时测定多种金属元素、检出限低、分析速度快、动态范围宽，在实际工作中大大地提高了工作效率，随着此仪器的逐步推广使用，已经越来越广泛应用于水、食品及生物材料等的分析。     

电感耦合等离子体质谱法同时测定化妆品中的铅、镉、砷

目的:建立同时检测化妆品中的铅、镉、砷的电感耦合等离子体质谱分析法。方法:以微波消解法对化妆品进行消解预处理后,以电感耦合等离子体质谱法进行检测。结果:铅、镉、砷浓度在0μg/ml～0.50μg/ml范围内相关系数r>0.999。铅、镉、砷的最低检出限分别为0.000023μg/ml、0.0000031μg/ml、0.000012μg/ml,以取1 g样品分析计,本法最低检出浓度铅、镉、砷分别为0.0006μg/g、0.00008μg/g、0.0003μg/g。样品加标回收率铅、镉、砷分别是92.7%～104.1%、91.7%～96.0%、95.9%～103.4%,铅、镉、砷的相对标准偏差均<2%。结论:本法具有良好的准确度和精密度,灵敏度高,检出限低,线性范围宽,干扰少,适应于不同样品基体中铅、镉、砷的测定。     

微波消解测定食品中铅、镉、砷、汞的方法探讨

[目的]通过对微波消解条件的最优化研究,以达到快速、简便、准确的测定食品中铅(Pb)、镉(Cd)、砷(As)、汞(Hg)。[方法]采用标准样品进行不同处理方法间的对比实验,来证明新方法的准确度、精密度满足现行标准要求。[结果]微波消解前处理,回收率和相对标准偏差(RSD)分别为Pb:89．3％-106．7％,6．87％;Cd:93．4％-116．2％,7．23％; As:89．2％-113．5％,9．05％;Hg:91．9％-111．2％,7．70％。与国标法比较差别没有显著性。[结论]微波消解技术具有快速、简便、准确的特点,是能适用于食品中微量元素测定前处理要求的新技术。     

微波消解-电感耦合等离子体质谱法测定大米中铅、镉、砷、汞、铬含量

目的 建立微波消解—电感耦合等离子体质谱法(ICP-MS)同时测定大米中铅、镉、砷、汞、铬含量,为新标准《食品安全国家标准食品中污染物限量》的实施提供方法参考。方法 样品经硝酸与微波消解处理,优化的ICP-MS条件,采用在线引入内标,对大米中5种重金属进行检测,同时用大米粉国家标准物质GBW(E)100349a对方法准确度、精密度进行验证。结果 通过对大米粉标准物质分析,所测的5种重金属元素测定值均在参考值范围内,大米样品3水平加标回收率为82%～108%,RSD为2.8%～7.5%。结论 根据国标GB 2762—2022规定的大米中5种重金属限值标准,本实验所测大米样品均未超过限值,合格率100.0%。该方法检测效率高,检出限低,检测结果快速、准确,适合大米中5种重金属元素同时分析测试。     

微波消解电感耦合等离子体质谱法测定土壤中铅、铬、镉

目的 建立硝酸-过氧化氢-氢氟酸微波消解电感耦合等离子体质谱法(ICP-MS)测定土壤中铅、铬、镉的方法.方法 将新鲜土壤样品晾晒过筛,混合酸微波消解定容后,选择钪、铟、铋为内标液,电感耦合等离子体质谱法(ICP-MS)测定样品中铅、铬、镉三种元素的含量.结果 三种元素的线性范围分别为:铅1.00～300.00μg/L...     

微波消解—碰撞反应池技术电感耦合等离子体质谱法测定食品中的铅

目的 建立食品中铅的微波消解—碰撞反应池技术电感耦合等离子体质谱法.方法 样品经微波消化后直接用碰撞反应池电感技术的耦合等离子体质谱仪(ICP-MS)进行测定.用铊(204TI)内标校正基体干扰和漂移,用高性能Xs接口降低非质谱干扰,用碰撞反应池技术(CCT模式)消除质谱干扰.结果 方法的标准曲线线性范围为0～40μg/L,相关系数为0.999 8.方法检出限为0.000 5mg/kg,最低检出浓度为0.001 7 mg/kg,相对标准偏差为1.1％～3.8％,回收率为93.3％～104.0％.结论 本方法灵敏、准确,操作简便、快速,对样品的测定结果与石墨炉原子吸收光度法之间无显著性差异,能用于食品中铅的准确测定.     

电感耦合等离子体质谱法同时测定居住区大气中痕量铅、镉

目的建立电感耦合等离子体质谱法测定居住区大气中有害痕量元素铅、镉的分析方法。方法通过超声浸提同时分离气溶胶样品中的铅、镉,对仪器工作参数进行优化,分别选取^115In、^204T1作为测定元素的校正内标,有效克服了基体效应、接口效应和仪器漂移对测定信号产生的影响。在优化的仪器条件下,取采样滤膜分别加入低、中、高浓度标准溶液进行测定,计算加标回收率。结果测定元素标准曲线的相关系数均优于0．9997,气溶胶样品中镉和铅测定的方法检测限分别为0．007ng／m^3和0．045ng／m^3,通过测定标准参考物质GBW（E）080212考察方法的准确性,测定值均在标准值范围内。镉和铅两种元素的加标回收率在94．6％～107．1％之间,测定精密度在1．2％～3．7％之间。结论该方法精密度、准确性好,简便、快速、灵敏,适用于居住区大气中痕量元素镉、铅含量的测定。     

密闭微波消解-电感耦合等离子体发射光谱法测定鱼肉中铅,镉和汞

目的:建立密闭微波消解-电感耦合等离子体发射光谱法测定鱼肉中的铅,镉和汞的方法。方法:样品碾磨泥状,加入硝酸,双氧水1,80℃密闭微波消解30 min,横向轴电感耦合等离子体发射光谱同时测定铅、镉和汞。结果:对四份样品进行测定,Pb,Cd和Hg的相对标准偏差<10%,加标回收率92%～101%。结论:本法快速、灵敏,准确度高,精密度好,适用于鱼基体中铅、镉和汞的测定。     

电感耦合等离子体质谱法测定苦丁茶中的铅、镉、砷、汞和铬

目的利用电感耦合等离子体质谱(ICP-MS)技术建立一种同时检测苦丁茶中铅、镉、砷、汞和铬的方法。方法采用硝酸-过氧化氢混合酸为消解溶剂,样品经微波处理后,应用ICP-MS法同时测定样液中的铅、镉、砷、汞和铬的含量。分别选用锗、铟、铋为内标元素,以校正实验过程中仪器信号的漂移和样品的基体效应。采用校准方程75As=-3.13220×40Ar37Cl对砷的检测结果进行校正。结果铅、镉、砷、汞和铬的线性相关系数均>0.999,方法检出限为0.003 mg/kg^0.007 mg/kg,方法精密度为3.1%~18.4%,加标回收率为88.2%~113.4%,标准物质菠菜(GBW10015)和绿茶(GBW10052)的检测结果与参考值相符合。结论本法快速简便,准确度和精密度均符合检测要求,适用于苦丁茶中铅、镉、砷、汞和铬的测定。     

济宁南四湖鸭肉中砷、铅、汞、镉含量调查

对湖区和工厂饲养的鸭子不同部位的砷、铅、汞、镉含量进行了检测,结果表明湖鸭铅、汞、镉的含量明显高于工厂饲养的家鸭(P<0.05);肝、背、脖3个部位的含量高于其它部位,同时对湖水及湖鸭的部分食用鱼、螺等进行了铅、砷、汞、镉的检测,结果湖水及所检食物均受到不同程度的污染,其中以汞污染较重。     

Genotypic differences in arsenic,mercury, lead and cadmium in milled rice (Oryza sativa L.)

The contents of arsenic, mercury, lead and cadmium in milled rice were determined. Among 216 genotypes, the As, Hg, Pb and Cd contents were ranged from 5.06 to 296.45, 2.46 to 65.85, 4.16 to 744.95 and 5.91 to 553.40 ng/g, respectively. Six genotypes with lower contents of toxic metal elements were selected. The averages of As and Pb contents for indica rice were higher than those of japonica rice, while the averages of Hg and Cd contents were in contrast. Compared with white brown rice, the milled rice from black and red brown rice contained lower contents of four elements. Significant negative correlation was found between As content and alkaline spread value. Significant correlations were observed between As and aspartic acid (Asp) content, Hg and Asp or leucine contents, Pb and cysteine or methionine contents. Cd content was significantly negatively correlated with protein and 14 amino acid contents.     

Associations of toenail arsenic, cadmium, mercury, manganese, and lead with blood pressure in the normative aging study

Background: Arsenic, cadmium, mercury, and lead are associated with cardiovascular disease in epidemiologic research. These associations may be mediated by direct effects of the metals on blood pressure (BP) elevation. Manganese is associated with cardiovascular dysfunction and hypotension in occupational cohorts.Objectives: We hypothesized that chronic arsenic, cadmium, mercury, and lead exposures elevate BP and that manganese lowers BP.Methods: We conducted a cross-sectional analysis of associations between toenail metals and BP among older men from the Normative Aging Study (n = 639), using linear regression and adjusting for potential confounders.Results: An interquartile range increase in toenail arsenic was associated with higher systolic BP [0.93 mmHg; 95% confidence interval (CI): 0.25, 1.62] and pulse pressure (0.76 mmHg; 95% CI: 0.22, 1.30). Positive associations between arsenic and BP and negative associations between manganese and BP were strengthened in models adjusted for other toenail metals.Conclusions: Our findings suggest associations between BP and arsenic and manganese. This may be of public health importance because of prevalence of both metal exposure and cardiovascular disease. Results should be interpreted cautiously given potential limitations of toenails as biomarkers of metal exposure.     

2013 - 2017年烟台市食品中镉、汞和砷的含量检测分析

目的 了解烟台市2 807份食品中镉、总汞和总砷的污染状况。方法 采用随机采样的方法于2013 - 2017年间采集烟台市售17类2 807份食品,依据国标规定的操作程序进行检测。结果 镉总体合格率为99.75%（2 770/2 777）。超标样品为6份梭子蟹和1份扇贝。藻类、水产品和食用菌镉含量较高,均值分别为0.756 mg/kg、0.0901 mg/kg和0.0487 mg/kg;乳及乳制品、水果及其制品和饮料镉含量较低,均值分别为0.000625 mg/kg、0.000142 mg/kg和未检出。总汞总体合格率为99.96%（2 666/2 667）。超标样品为1份姬松茸（干制品）。水产品、藻类和食用菌总汞含量较高,均值分别为0.0761 mg/kg、0.0310 mg/kg和0.0106 mg/kg。蔬菜及其制品、水果及其制品和饮料总汞含量较低,均值分别为0.000272 mg/kg、0.000195 mg/kg和未检出。总砷总体合格率为100%（2 677/2 677）。藻类、水产品和食用菌总砷含量较高,均值分别为35.410 mg/kg、1.0087 mg/kg和0.0575 mg/kg。豆类、蛋类和饮料总砷含量较低,均值分别为0.00467 mg/kg、未检出和未检出。2013 - 2017年镉检出率分别为77.84%、61.90%、62.06%、31.52%和28.33%。2013 - 2017年总汞检出率分别为13.77%、15.00%、29.76%、9.69%和14.44%。2013 - 2017年总砷检出率分别为14.77%、7.38%、45.57%、11.50%和12.68%。结论 烟台市2 807份食品中镉、总汞、总砷的污染水平较低。     

铅、镉、砷污染地区人群免疫功能检测分析

目的探讨铅锌矿矿区铅镉砷混合接触对不同暴露人群机体免疫状况的影响。方法选择铅锌矿矿区矿工、矿区居民和无污染地区居民3组人群共96人作为研究对象,对3组人群所处环境中的铅、镉、砷含量,人体血液和尿液的铅、镉、砷含量以及人体免疫学指标进行分析。结果矿工组血中铅、镉、砷含量几何均数分别为216.57,5.04,58.65μg/L,矿区居民组血中铅、镉、砷含量几何均数分别为143.62,2.42,33.24μg/L,均高于对照人群,几何均数分别为81.54,1.18,11.50μg/L(P<0.01)。3组人群尿液中的各种毒物差异有统计学意义(P<0.01)。矿工和矿区居民的免疫功能相对于对照组均有不同程度的下降(P<0.01)。结论接触铅、镉和砷的矿区矿工和居民免疫功能受到了不同程度的损害。     

食品中痕量铅检测的氢化物发生-原子荧光法的改进

目的:建立一种简便准确的氢化物发生-原子荧光光谱法检测食品中的痕量铅的方法。方法:采用干法消解样品,在酸性介质中,以铁氰化钾为氧化剂,2%的盐酸为载流,样品中的铅与硼氢化钠(NaBH4)或硼氢化钾(KBH4)反应生成铅的挥发性氢化物(PbH4),将氢化物导入原子化器中,检测其荧光强度。结果:铅在0.00μg/L~50.0μg/L范围内,荧光强度值与铅浓度相关系数r>0.9990,检出限为0.094μg/L,相对标准偏差0.80%~4.70%,加标回收率82.1%~104.0%。结论:应用改进后的氢化物发生-原子荧光法检测食品中痕量铅,具有操作简便、线性关系好、检出限低、重复性好、回收率高、结果准确的优点,且分析成本低廉,便于推广应用。     

Assessing arsenic,cadmium, and lead contents in major crops in Brazil for food safety purposes

The food chain is one of the major sources of human exposure to non-essential trace elements (TEs) present in soils. Human exposure to contaminated food is a worldwide health concern and a food safety issue that threatens agricultural trade. To assess the quality of Brazilian food products with respect to non-essential TEs, we evaluated arsenic (As), cadmium (Cd), and lead (Pb) contents in five major crops grown in Brazil: rice, wheat, corn, soybeans, and potatoes. The samples were collected from field trials with a record of long-term use of phosphate fertilizers in the states of Mato Grosso and Minas Gerais, Brazil. The TE concentrations in soils were all bellow the maximum allowable concentrations for agricultural soils. The mean concentrations of As, Cd, and Pb (μg kg⁻¹ dry weight) were as follows: below the detection limit <15, 29, and <40 for rice; 19, 23, and 64 for wheat; 47, 40, and 95 for corn; 65, 23, and 106 for soybeans; and 59, 22, and <40 for potatoes, respectively. Significant differences were found in the As and Cd contents of the different wheat cultivars. The levels of As, Cd, and Pb found in the studied crops are well below the values reported in the literature and are in accordance with the Codex Alimentarius and the European Union and Brazilian guidelines, indicating that the concentrations of these elements in the crops do not pose a risk to human health.     

微波消解-氢化物发生原子荧光光谱法同时测定食品中汞和砷

目的:建立微波消解-氢化物发生原子荧光光谱法同时测定食品中汞和砷的方法。方法:食品样品经微波消解后,用氢化物双道原子荧光光谱法同时测定食品中汞和砷的浓度。结果:本法在汞浓度为0μg/L～1.0μg/L、砷浓度为0μg/L～10μg/L范围内有良好的线性关系,相关系数rHg=0.9998,rAs=0.9997,检出限为Hg:0.0002 mg/kg,As:0.005 mg/kg;相对偏差为Hg:1.2%,As:0.83%;回收率为Hg:85%～91%,As:94%～103%。结论:该方法具有简便、快速、灵敏度高等优点,适合日常批量检测。     

Reference intervals of cadmium,lead, and mercury in blood,urine, hair,and nails among residents in Mansoura city,Nile delta,Egypt

A random sample of 68 males and 25 females who reside in Mansoura city, Egypt, was examined for concentrations of cadmium, lead, and mercury in blood, urine, hair, and nails. The effect of gender and smoking on such levels was studied. The influence of dental amalgam on the levels of mercury in these biological samples was also examined. The results obtained show that only blood lead, which increased among males, was affected by gender. Blood levels of cadmium and lead as well as hair lead appeared to increase with smoking habit. Mercury levels in blood and urine were related to the presence of dental amalgam fillings. International comparisons between our results and the corresponding levels in other localities in the world showed that there were environmentally related variations in terms of cadmium levels in hair, lead levels in blood, urine, hair, and nails, and mercury levels in blood, hair, and nails. In conclusion, reference intervals of cadmium, lead, and mercury in the biological samples are environmentally related parameters. Some factors, such as gender, smoking habit, and the presence of dental amalgam fillings, may affect such levels and therefore should be considered.     

微波消解同时测定农产品中铅、镉、汞

目的:建立一种适合同时测定农产品中铅,汞,镉的样品前处理方法。方法:采用微波消解方法处理样品,样品消化液经赶酸后定容,分别用来测定汞和铅、镉。结果:测定铅,镉,汞方法的线性范围分别为:0.0μg/L～20μg/L,0.0μg/L～2μg/L,0.0μg/L～5μg/L;相关系数分别为:0.9979,0.9978,0.9988;回收率分别为:95.8%～103%,95.1%～104%,98.4%～110.6%;方法的检测限分别为0.012μg/L,0.009μg/L,0.0027μg/L。结论:该方法精密度好,准确度高,快速简单,能够很好地满足农产品中铅,汞,镉含量的测定要求。