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...     

快速湿法消解-电感耦合等离子体质谱法同时测定紫菜中铅、砷、汞、镉含量

目的建立测定紫菜中的铅、砷、汞、镉含量的快速湿法消解-电感耦合等离子体质谱测定方法。方法紫菜样品用硝酸在石墨消解仪上120℃消解30 min,冷却后用去离子水定容。采用电感耦合等离子体质谱法测定紫菜样品中的铅、砷、汞、镉的含量。结果将紫菜标准物质(GBW 10023)和实际样品用快速湿法消解和微波消解法进行消解,检测结果基本一致,均与证书参考值吻合。本实验铅、砷、镉在0μg/L～30μg/L,汞在0μg/L～5μg/L时,线性关系良好(相关系数为0. 999 6～1. 000 0),检出限为0. 002 6 mg/kg～0. 047 mg/kg,相对标准偏差为2. 5%～7. 3%。结论快速湿法消解简化了前处理操作流程,最大程度上提高了前处理的工作效率,更适合于大批量样品的前处理。快速湿法消解-电感耦合等离子体质谱法同时具有操作简便、快速、结果可靠等优点,适合于紫菜中铅、砷、汞、镉的快速检测。     

应用电感耦合等离子体质谱法测定紫菜、海带中铅、镉含量

目的:应用电感耦合等离子体质谱法(ICP-MS)测定紫菜、海带中铅、镉含量。方法:用微波消解进行样品前处理,以In,Bi作内标,采用电感耦合等离子体质谱法测定紫菜、海带中铅、镉含量。结果:线性范围宽,相关系数大于0.999;方法的相对标准偏差小于等于6%;方法的准确度:选择美国标准物质牡蛎(NBS1566)、贻贝(GBW08571),分别测定Pb、Cd含量,测定值均在标准值范围内。结论:电感耦合等离子体质谱法(ICP-MS)测定紫菜、海带中铅、镉含量,方法简单、快速、灵敏度高、线性范围宽、干扰少。     

ICP-AES测定花粉中10种微量元素的方法研究

目的建立花粉中10种微量元素的测定方法。方法采用微波消解法处理样品,电感耦合等离子体原子发射光谱化(ICP-AES)法测定铬、锌、铜、锰、砷、铁、铅、镉、硒和铝10种微量金属元素。结果 ICP-AES——微波消解法回收率为:93.2%～107.8%,相对标准偏差为1.58%～3.44%。结论 ICP-AES——微波消解法具有简便、快速、准确等特点,适用于花粉中10种微量金属的测定。     

电感耦合等离子体-质谱法测定婴幼儿食品中铅镉汞砷

目的 为保障婴幼儿食品的质量安全,建立婴幼儿食品中铅镉汞砷的电感耦合等离子体-质谱法并对石家庄市各个品牌的婴幼儿食品中铅、镉、汞、砷进行安全风险监测。方法 按照国家食品污染和有害因素风险监测工作手册方法:经微波消解处理,采用电感耦合等离子质谱(ICP-MS)测定;按照国家食品安全相关标准对检测结果进行卫生学评价。结果 在2013年所检测的70份样品中,铅、镉、汞和砷总检出率分别是11.4%、27.1%、0%、0%,总合格率分别是92.8%、100.0%、100.0%和100.0%,样品中除铅外,其他重金属的含量均无超标现象,但部分婴幼儿食品仍检出微量重金属。结论 石家庄市市售婴幼儿食品重金属污染较轻,食品污染物风险监测应该继续加强。     

微波消解ICP-MS和GFAAS测定中药材中铅镉含量的对比研究

目的:运用电感耦合等离子体质谱法(ICP-MS)和石墨炉原子吸收光谱法(GFAAS)测定几种中药材中铅、镉的含量,并对结果进行比较。方法:微波消解前处理样品,分别采用石墨炉原子吸收光谱法(GFAAS)和电感耦合等离子体质谱法(ICP-MS)测定样本中铅、镉含量。结果:ICP-MS线性关系均大于0.9994,GFAAS线性关系均大于0.9991,精密度(RSD)为3.1%～4.9%,国家标准物质:丹参(GBW(E)090066)、黄芪(GBW09588),两种方法检测结果均在范围之类,不存在显著性差异。结论:微波消解—电感耦合等离子体质谱法(ICP-MS)和石墨炉原子吸收光谱法(GFAAS)均可用于测定中药材中铅、镉含量,ICP-MS能同时测定多种元素,但仪器昂贵且维护成本高,GFAAS测量方法简便、精度高,但每一元素需要分别测定,且干扰较大。     

微波消解等离子体质谱法测定各类食品中痕量汞、镉、铅、砷准确性探讨

目的 建立微波消解-电感耦合等离子体质谱法（ICP-MS）准确测定各类食品中痕量汞、镉、铅、砷的分析方法。方法 采用微波消解法处理样品,ICP-MS测定以^72Ge、^103Rh、^185Re作为内标消除非质谱干扰,八极杆碰撞池（ORS^3）消除质谱干扰。结果 采用本方法测定汞、镉、铅、砷的定量限分别为0.05、0.05、0.40、0.40μg/L;在定量限附近测定的回收率和相对标准偏差分别为：100.0%、90.0%、96.0%、112.0%和7.6%、8.0%、11.8%、6.2%。结论 采用ICP-MS法准确测定食品中痕量有害元素的关键点及控制措施,适用于食品安全风险监测大批量样品的分析。     

微波消解-八极杆碰撞模式-电感耦合等离子体质谱法检测花生中6种重金属

目的 建立微波消解-八极杆碰撞模式-电感耦合等离子体质谱法(ORS-ICP-MS)同时测定花生中铬(Cr)、镍(Ni)、砷(As)、镉(Cd)、铅(Pb)和汞(Hg)6种重金属含量.方法 样品去壳粉碎均匀,称取0.3500 g于消解罐中,加入5 mL硝酸和1 mL过氧化氢消解体系,经微波消解后以纯水定容,在线加入内标元...     

微波消解ICP-MS法测定山茱萸中5种重金属的含量

建立电感耦合等离子体(ICP-MS)法测定山茱萸药材中铜、镉、汞、铅和砷含量的方法。山茱萸样品经微波消解法处理,补偿基体效应,采用ICP-MS法同时测定上述5种重金属元素。对于所测元素,校准曲线相关系数r>0.9994,回收率均在96.8%～104.0%,RSD<5.6%。方法准确、简便、快速、灵敏,可用于山茱萸中重金属的含量测定。     

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。     

Metal pollution as health indicator of lake ecosystems

As part of a long-term monitoring study of the anthropogenic pollution of the Lake of Balaton (Hungary) the concentrations of toxic metals (Cd2+, Hg2+, Pb2+), as well as of bioelements (Cu2+ and Zn2+) were measured in the muscle, gill and liver of bream (Abramis brama L.) collected in the open water during the autumn of 1999, The highest Cd, Cu, Pb and Zn concentrations were detected in the gill and liver of fish, whereas the highest Hg concentrations were measured in the muscle. The maximum metal concentrations measured in the muscle of bream were generally below maximum permissible levels for human consumption established by the Hungarian Food Directorate. Depending on the sampling site, significantly higher Cd, Hg and Pb concentrations (p < 0.05) were detected in the muscle of fish samples collected from the Western basin, while no significant differences were observed for Cu and Zn. In the muscle and gill an increasing trend of heavy metal (Cd and Cu) load characterizes the individuals of the 2-4 calendar age group (p < 0.05), while for the older specimens the concentration of these elements decreased significantly (p < 0.05). Positive relationships on the whole age scale were found for Cd in the liver, for Pb in the gill, and for Hg both in the muscle and the liver of fish.     

Metal Analysis of Scales Taken from Arctic Grayling

This study examined concentrations of metals in fish scales taken from Arctic grayling using laser ablation–inductively coupled plasma mass spectrometry (LA-ICPMS). The purpose was to assess whether scale metal concentrations reflected whole muscle metal concentrations and whether the spatial distribution of metals within an individual scale varied among the growth annuli of the scales. Ten elements (Mg, Ca, Ni, Zn, As, Se, Cd, Sb, Hg, and Pb) were measured in 10 to 16 ablation sites (5 μm radius) on each scale sample from Arctic grayling (Thymallus arcticus) (n = 10 fish). Ca, Mg, and Zn were at physiological levels in all scale samples. Se, Hg, and As were also detected in all scale samples. Only Cd was below detection limits of the LA-ICPMS for all samples, but some of the samples were below detection limits for Sb, Pb, and Ni. The mean scale concentrations for Se, Hg, and Pb were not significantly different from the muscle concentrations and individual fish values were within fourfold of each other. Cd was not detected in either muscle or scale tissue, whereas Sb was detected at low levels in some scale samples but not in any of the muscle samples. Similarly, As was detected in all scale samples but not in muscle, and Ni was detected almost all scale samples but only in one of the muscle samples. Therefore, there were good qualitative and quantitative agreements between the metal concentrations in scale and muscle tissues, with LA-ICPMS analysis of scales appearing to be a more sensitive method of detecting the body burden of Ni and As when compared with muscle tissue. Correlation analyses, performed for Pb, Hg, and Se concentrations, revealed that the scale concentrations for these three metals generally exceeded those of the muscle at low muscle concentrations. The LA-ICPMS analysis of scales had the capability to resolve significant spatial differences in metal concentrations within a fish scale. We conclude that metal analysis of fish scales using LA-ICPMS shows considerable promise as a nonlethal analytical tool to assess metal body burden in fish that could possibly generate a historic record of metal exposure. However, comprehensive validation experiments are still needed. Received: 8 March 2000/Accepted: 31 May 2000     

Dietary Intake of Toxic Heavy Metals with Major Groups of Food Products—Results of Analytical Determinations

Food contains a complex matrix of various substances, including essential nutrients, non-nutritive substances, and toxins, including metals. The main purpose of the study was to evaluate the contribution of major groups of food products to an overall intake of toxic heavy metals (Cd, Pb, Hg, and Ni) using a combination of the 24-dietary recall technique, the ICP-OES (Inductively Coupled Plasma Optical Emission Spectrometry) method, and chemometric tools. The obtained results reveal that there is a high potential risk of developing nephrotoxicity through the dietary intake of Pb in the case of both genders. The dietary intake determined for other elements (Cd, Hg, and Ni) was far below the limits established by European Food Safety Authority (EFSA). Principal Component Analysis (PCA) supported analytical determinations and revealed that cereals and vegetables were major contributors to a total intake of Cd (39.6 and 17.4% of the total exposure, respectively), Ni (40.4 and 19.3%), and Hg (16.8 and 19.6%), while water and beverages were major dietary sources of Pb (31% of the total daily intake). In contrast, eggs, fats and oils, and milk and dairy products provided the smallest amounts of Cd, Pb, and Ni. Despite containing high amounts of Hg, considering very low consumption, fish were not found to be an important source of this element.     

Nutritional Quality and Safety Related to Trace Element Content in Fish from Tyrrhenian Sea

This study analyzed for the detection of the following trace elements: As, Cd, Cu, Hg, Pb, Se, Zn, in muscle of four widely traded and consumed marine fish species (Mullus surmuletus L., Merluccius merluccius L., Micromesistius poutassou (Risso, 1827), Scomber scombrus L.) selected for their wide trade and consumption. Mean concentrations found in fish muscle, irrespective of species, ranged from 3.61 to 105.49 (As); 0.01–0.08 (Cd); 0.74–4.71 (Cu); 0.09–1.10 (Hg); 0.02–0.58 (Pb); 0.30–2.88 (Se); 11.56–73.37 (Zn) mg/kg wet weight. As, Hg, Cu and Se concentrations showed a significant difference (p < 0.01) among the analyzed species in winter and in summer. Cd exhibited a significant difference (p < 0.01) only in summer. The maximum levels set for Hg, Cd and Pb by European Regulation No 1881/2006 were exceeded by 5 (8.9 %), 1 (1.8 %) and 4 (7.1 %) samples, respectively. In particular the species exceeding the legal limits were red mullet for Cd and Pb, Atlantic mackerel and blue whiting for Hg and Pb.     

Mercury, cadmium and lead levels in Bagrus bayad fish from the river Nile, Delta Region, Egypt

A total of 50 random samples of Bagrus bayad were collected from various localities of River Nile at lower Egypt and were analyzed for determination of Hg, Cd and Pb concentrations by AAS. The obtained results revealed that the concentrations of Hg, Cd and Pb in fish muscles were ranged from 0.026 to 0.391, 0.028 to 0.053 and 0.022 to 0.654 with mean +/- SE values of 0.190 +/- 0.017, 0.048 +/- 0.003 and 0.215 +/- 0.047 microg/g wet weight, respectively. 24% and 6% of the examined fish samples exceeded the maximal permissible limit set by FAO/WHO (1992) for Cd and Pb, respectively. Whereas none of the examined samples exceeded the maximal limit for Hg. The possible health hazards of heavy metals as well as the suggestive measures for minimizing the pollution of fish and water had been discussed.     

Heavy Metal Concentrations in Food Chain of Lake Velenjsko jezero, Slovenia: An Artificial Lake from Mining

The concentration of metals (Pb, Cd, Zn, Hg) in different ecosystem components (lake water, sediment, plankton, macrophytes, and fish tissues) has been determined in Velenjsko jezero, an artificial lake resulting from mining activity. The risk to humans from consuming fish has been evaluated from the heavy metal load of fish muscle tissue. Heavy metals are transferred through the food chain at different levels, and Hg is found to be the element of the highest ecotoxicological concern. Although both sediment and plankton contain relatively low concentrations of Hg, this element accumulates in high levels in fish, especially in the benthivorous species Abramis brama danubii and predator species Perca fluviatilis. Moreover, Hg appears to be very mobile in the fish organism. Whereas the other metals remained mostly in liver (Cd) or gills (Zn, Pb), levels of Hg in fish muscle and liver were the same and markedly higher than in gills. However, in muscle, the average concentrations of each metal were below their maximum limits, determined either by Slovenian legislation or by the Food and Agriculture Organization.     

Assessment of trace elements in canned fishes (mackerel, tuna, salmon, sardines and herrings) marketed in Georgia and Alabama (United States of America)

The concentrations of mercury and 13 other trace metals in 104 canned fish samples purchased within the states of Georgia and Alabama (United States of America) were determined using the direct mercury analyzer (DMA) and the inductively coupled plasma-optical emission spectrometer (ICP-OES). The ranges obtained for the elements analyzed in mg/kg (wet weight) are as follows: Hg (0.02–0.74), Ag (0.0–0.20), As (0.0–1.72), Cd (0.0–0.05), Cr (0.0–0.30), Fe (0.01–88.4), Pb (0.0–0.03), Mn (0.01–2.55), Ni (0.0–0.78), Co (0.0–0.10), Cu (0.01–5.33), Sn (0.04–28.7), V (0.0–0.31) and Zn (0.14–97.8). Three tuna samples had Hg level above the European dietary limit of 0.5 mg Hg/kg. The mean Hg concentrations in the tuna (285 μg/kg) and sardine (107 μg/kg) brands were higher than the averages posted by the pink salmon (36.1 μg/kg), red salmon (32.8 μg/kg) and mackerel (36.4 μg/kg) brands. Two tuna samples and a sardine sample exceeded the Australian permissible limit of 1 μg/g inorganic arsenic (wet weight). Two samples (brand 15: herring) had zinc levels exceeding the Food and Agriculture Organization (FAO) recommended limit of 40 mg/kg and two pink salmons also exceeded the Brazilian regulatory limit of 0.1 mg Cr/kg. One tuna sample had a cadmium level slightly exceeding the Codex Committee on Food Additives and Contaminants draft guideline of 0.50 mg Cd/kg. However, the concentrations of lead, cadmium and copper were below the corresponding MAFF guidelines of 2.0, 1.0 and 30 mg/kg, respectively. Also, based on the United States Environmental Protection Agency (US EPA) health criteria for carcinogens, there are no health risks with respect to Pb, Cr, Cu and Zn concentrations in canned fishes analyzed. The result of the one-way analysis of variance (ANOVA) conducted on the data suggested that significant variations (P<0.05) existed in the concentrations of Hg, As, Co, Cr, Cu, Fe, Mn, Sn, V, and Zn across the various fish species and canned fish brands analyzed. The estimated weekly intakes of Hg, As, Cd, Pb, Sn, Fe, Cu and Zn for a 60 kg adult consuming 350 g of fish/week were below the respective provisional tolerable weekly intakes (PTWI) in μg/kg body weight for: Hg: 5; As: 15; Cd: 7; Pb: 25; Sn: 14000; Fe: 5600; Cu: 3500; and Zn: 7000.     

Biomonitoring of mercury,cadmium, and lead exposure in Japanese children: a cross-sectional study

Objectives

To measure current Hg, Cd, and Pb exposure in Japanese children, and to estimate dietary intakes of foods responsible for high body burden.

Methods

Blood, hair, and urine samples were collected from 9 to 10-year-old 229 children in Asahikawa and measured for Hg, Cd, and Pb in these matrices. Diet history questionnaire was used to estimate intake of marine foods and other food items. Hg level was measured by cold vapor atomic absorption spectrometry. Cd and Pb levels were determined with inductively coupled plasma mass spectrometry.

Results

Geometric mean (GM) of blood Hg, Cd, and Pb was 4.55 μg/L, 0.34 μg/L, and 0.96 μg/dL, respectively. Urinary Cd level was 0.34 μg/g creatinine (GM) and hair Hg was 1.31 μg/g (GM). Approximately one-third (35 %) of blood samples had Hg level above the U.S. EPA reference dose (RfD; 5.8 μg/L). Hair Hg level exceeded U.S. EPA RfD (1.2 μg/g) in 59 % samples. Children in the upper quartile of blood Hg level had significantly higher intake of large predatory fish species compared to those in the lower quartile of blood Hg.

Conclusions

Those with high blood Hg level may be explained by more frequent intake of big predatory fish. Cd and Pb exposure is generally low among Japanese children. As no safety margin exists for Pb exposure and high exposure to MeHg is noted in Japanese population; periodic biomonitoring and potential health risk assessment should continue in high-risk populations, notably among children.     

Human exposure in Italy to lead,cadmium and mercury through fish and seafood product consumption from Eastern Central Atlantic Fishing Area

The presence of cadmium (Cd), lead (Pb) and mercury (Hg) was investigated in fish and seafood products collected from the FAO Major Fishing Area 34, Eastern Central Atlantic. Samples were purchased from different retail outlets in Italy. Samples were selected so as to assess human exposure through diet. Metals were detected by Q-ICP-MS and Hg-AAS. All the metal concentrations detected were largely below the maximum levels (MLs) established by the European Union. The exposure assessment was undertaken by matching the concentration of Cd, Pb and total Hg in fish and other seafood products selected purposed according to Italian consumption data. The estimated weekly intakes (EWIs) for the evaluated elements related to the consumption of fish and other seafood products by the median of the Italian total population accounted for 14%, 2% and 14% of the standard tolerable weekly intake (TWI) for Cd and Hg as well as the provisional tolerable weekly intake (PTWI) for Pb, respectively.     

Concentrations of Trace Elements in Tissues of Red Fox (Vulpes vulpes) and Stone Marten (Martes foina) from Suburban and Rural Areas in Croatia

Trace elements concentrations (As, Cd, Cu, Pb and Hg) were determined in the liver, kidney and muscle of 28 red fox (Vulpes vulpes) and 16 stone marten (Martes foina) from suburban and rural habitats from Croatia. Rural and suburban habitats affected Cd and Hg levels in the muscle, liver and kidney of red fox. Significant differences in metal concentrations in the muscle, liver and kidney were detected among species. Suburban stone marten accumulated the highest levels of trace elements (mg/kg w.w.): in muscle 0.019 for Hg; in liver 0.161 for Cd, 36.1 for Cu and 0.349 for Pb; in kidney 1.34 for Cd and 0.318 for Pb. Values observed were higher than those found in suburban red fox and therefore, may represent an important bioindicator for the accumulation of toxic metals in urbanized habitats.