微波消解/ICP-MS法同时测定贝类产品中16种金属元素的含量

本文建立了微波消解-电感耦合等离子体质谱(ICP-MS)同时测定贝类产品中Cr、Mn、Fe、Co、Ni、Cu、Zn、As、Se、Mo、Ag、Cd、Ba、Hg、Tl和Pb等16种金属元素含量的方法.采用微波消解法对样品进行消解,通过在线加入内标校正基体效应,利用ICP-MS测定贝类产品中16种金属元素的含量.测定元素校正曲线的相关系数均在0.9992以上,检出限为6.64× 10-4 ～0.0851 μg· L-1.对牡蛎样品平行测定6次,各元素相对标准偏差(RSD)均小于5％.利用该方法分析了标准参考物质扇贝(GBW10024)中的16种金属元素,其测定值与参考值吻合.该方法具有快速、简单、精密度和准确性良好等优点,适用于贝类产品多种金属元素的同时测定.     

全自动消解-石墨炉原子吸收光谱法测定海洋生物体中Pb和Cd

<正>以全自动消解-石墨炉原子吸收光谱法测定海洋生物体中Pb和Cd含量的方法。使用全自动消解仪消解海洋生物体后制备待测溶液,用石墨炉原子吸收光谱法测定海洋生物体中Pb和Cd的含量。实验证明,本方法的线性相关系数均大于0.9995,Pb和Cd的相对标准偏差均小于5%。方法简便、重现性好,适用于批量海洋生物体样品中Pb和Cd的测定。     

鄱阳湖短颌鲚体内矿物元素含量变化分析

为了解鄱阳湖短颌鲚体内矿物元素的分布状况,以评价其食用卫生质量以及为丰富短颌鲚研究提供基础性资料,采用火焰发射法和石墨炉原子吸收光谱法,测定了鄱阳湖短颌鲚全鱼中的常量元素(Na、K、Mg、Ca)和微量元素(Fe、Mn、Cu、Zn),以及微量重金属元素(Pb、Cd、Cr)的含量,分析了矿物元素在鱼体内的富集状况,并与刀鲚、湖鲚、凤鲚体内的矿物元素含量进行比较分析。结果表明:鄱阳湖短颌鲚体内所含的11种元素中,常量元素中K的含量最高,微量元素中Cu的含量最低。总体上,鄱阳湖短颌鲚含有丰富的矿物元素且符合我国规定的限量标准,属于可安全食用范围。     

微波消解ICP-MS法测定石油污染对虾体内16种元素含量的影响

采用电感耦合等离子体质谱法测定石油污染水体和非石油污染水体虾16种元素的含量。样品经微波消解,通过在线加入内标校正基体效应和接口效应,以修正方程校正质量数干扰,测定元素校正曲线的相关系数均在0.9994以上,方法检出限小于1.83μg/L,精密度优于5.98%,加标回收率为80.5%~119.8%。结果显示,石油污染影响到虾体内多种元素的含量,石油污染水体虾的Cr、Mn、Fe、Co、Ni、Zn、Cu、As、Se、Cd、Pb含量均明显高于非石油污染水体虾,差异均有统计学意义(P0.05)。石油污染水体虾的Mg、Al、Ca、Ag、Hg与非石油污染水体虾比较,差异均无统计学意义(P0.05)。同时也表明,电感耦合等离子体质谱法适于海产品中多种元素的检测,可以为海产品的质量控制和安全评价提供科学依据。     

石墨炉原子吸收法对水产品中硒的测定及不确定度评价

建立了水产品中硒的微波消解与石墨炉原子吸收光谱法的测定及不确定度评定方法。采用HNO_3-H_2O_2微波消解与石墨炉原子吸收光谱法,测定水产品中硒元素的含量。结果表明,该方法线性良好,相关系数大于0.999,检出限为0.030 mg/kg。在0.2、0.4、0.8 mg/kg 3个加标水平下的平均回收率为82.1%~87.7%,相对标准偏差为1.8%~7.8%。该方法灵敏度高、准确性好、简单易行,满足水产品中硒的检测要求,可显著提高分析效率。同时建立了石墨炉原子吸收法测定水产品中硒的不确定度评定方法,对测量过程中各不确定度分量进行分析和计算,得出合成标准不确定度和扩展不确定度。结果表明,该方法测定过程的不确定度主要来源于标准曲线校准、测试过程的随机效应及样品前处理。在实际操作中可用于指导检测质量的控制,对提高测定结果的准确性和可靠性有重要意义。     

日本鳗鲡幼体的耳石微化学分析及其环境指示元素筛选

在长江口日本鳗鲡鳗苗捕捞汛期,于长江靖江段采集日本鳗鲡幼体,采用同步辐射X射线荧光(XRF)定量分析方法测定了幼体矢耳石中14种元素的含量,分析了在海洋与淡水早期生活史阶段的微化学特征。结果显示,耳石中Ca和Sr为常量元素,Ba、Fe、Mn、Zn的含量也在1-10μg/g之间,Cr、Ni、Se、Co、Cu、Au则在1 mg/g以下。Ni、Cu、Mn、Cr、Co、Zn和Sr含量的稳定性较好,变异系数在30%以下;Se、Au的含量低且极不稳定,变异系数达40.8-75.0%;Fe在不同个体间存在显著的含量差异(p=0.007<0.05),但其他元素不存在个体差异。在海洋生活史阶段,Mn、Se、Co、Ba为强富集元素(BCFa-e >1000),Sr、Fe、Zn、Ni、Cu为中等富集元素(BCFa-e在100~1000)。除Sr、Ba和Se外,卵黄囊期和柳叶鳗期的耳石富集系数并无显著差异(p>0.05)。在淡水生活史阶段,Sr和Co为强富集元素(BCFa-e >1000),Se、Zn、Cu、Ba、Mn为中等富集元素(BCFa-e在100~1000),Ni、Fe为低富集元素(BCFa-e在10~100)。与海水阶段相比,耳石在淡水阶段的Fe、Ba、Mn、Se、Co、Ni富集系数均大幅减小,而对Sr、Zn、Cu的富集能力有所增大。分析表明,耳石内的Sr、Ba、Ni、Co为环境强响应元素,Fe和Mn为环境弱响应元素,Zn、Cu和Se为环境负响应元素,幼鳗自海洋至淡水的迁徙过程中,前者存在明显的时滞效应,但后两者的日间含量波动较大,缺乏响应的规律性。本文认为,用作鱼类迁移行为或栖息地环境变化的指示元素,需要具备耳石富集效应强、时滞效应小、不同环境间含量差异大、稳定性好、且为非必需元素等特点。从本研究结果看,只有Sr和Ba两种元素符合这些条件 。     

微波消解 — 原子光谱法测定海洋生物体中砷和镉

应用优化后的微波消解—原子光谱法测定6种海洋生物体标准物质中砷和镉元素含量,其中,使用原子荧光光谱法测定砷,石墨炉原子吸收光谱法测定镉,并评估测试结果的准确度和精密度.实验结果表明,砷和镉分别在1.0～20.0和0～5.0μg/L范围内有良好的线性关系,其线性相关系数均在0.9995以上,测定结果的准确度和精密度令人满...     

不同产地鲍鱼特征元素分析与主成分评价模型的建立

为了找出不同产地鲍鱼(Haliotis Spp.Abalone)的区域性差异,并探究一种有效的鲍鱼产地的鉴别方法,采用主成分分析法对对广东、福建、山东、辽宁4个主要养殖省份鲍鱼样品肌肉中的特征元素(Na、K、Mg、Ca、Fe、Zn、Cu、Ni、As、Al、Mn、Cr、Se)进行分析。结果显示,鲍鱼样品的元素含量存在差异,Mn的变异程度最大,变异系数为74%,Ni次之,为65%,其次是Se (60%),其余元素的变异系数均高于10%。同时,通过对这些数据进行降维处理,有效地从13个特征元素中提取了6个元素作为主成分,累计方差贡献率达89.87%;同时发现Ca、Se、Na、Fe、Mn、K、Ni这7种元素是不同产地鲍鱼的特征元素,并建立了主成分综合评价模型:F=0.2777F_1+0.2652F_2+0.1295F_3+0.1066F_4+0.0656F_5+0.0541F_6。模型的建立可以为利用特征元素对不同产地鲍鱼的产地溯源提供一定的理论参考。     

贝类体内重金属含量测定方法的研究进展

本文通过比较常见的国际上检测贝类体内重金属元素含量的方法,如石墨炉原子吸收法、火焰原子吸收法、电感耦合等离子体质谱法和原子荧光法等的准确度、精密度、检测周期等,对比4种方法的优点、缺点、适用的样本及范围,展望贝类重金属元素含量检测方法的发展趋势,为科学选择检测方法和手段提供参考。     

原子荧光法联测海洋生物中砷和汞方法的改进

本文运用微波消解,对原子荧光法联测海洋生物中砷和汞的方法进行改进,对仪器条件、微波消解体系、还原剂硼氢化钾浓度等条件进行优化,消除亚硝酸根（NO2）对测定的干扰。本方法经研究改进后,砷和汞的检测限分别为0．02mg／Kg和0．002mg／Kg;相对标准偏差分别为2．83％和2．05％;通过分析验证,改进后的方法简单、灵...     

几种海洋药用动物中重金属元素的含量分析

对我国几种传统海洋药用动物中重金属元素的含量进行了测定,并对同产地的陆生药用动物蛤蚧进行比较研究,其中Hg和As利用原子荧光光度计测定,Pb、Cd、Cu、Fe、Mn、Zn利用原子吸收光度计测定,样品采用微波消解仪消解。结果表明:海钱、海蛇、海马、海星的镉含量较高,海燕、海马、海星的铅含量较高,除个别样品微量元素未检出外,样品中Fe、Mn、Zn的含量相对较高。最后对金属元素含量较高的原因及对所含微量元素的食用安全性和营养学评价进行了探讨。     

Accumulation of Heavy Metals in the Nauplii of Artemia salina

Artemia salina cysts (San Francisco Bay Brand) were exposed in seawater containing multiple concentrations of either a single heavy metal (Hg, Cu, Zn, Pb, Cd, Co, Ni, Cr, Mn and Fe) or combination of heavy metals. The heavy metal accumulation in Artemia nauplii increased linearly with an increase in the heavy metal concentration in water. The metals could be detected in nauplii exposed to a single heavy metal at dosages of 5 μg/L for Hg, Zn, Mn, Fe and Cu; 25 μg/L for Cd and Cr; 50 μg/L for Co; 100 mUg/L for Ni; and 250 μg/L for Pb. Cysts exposed to several heavy metal combinations had minimum effective dosages equal to or lower than the single heavy metals- 5 μg/L for Cu, Cr, Zn, Mn and Fe; 25 μg/L for Cd and Ni; 50 μg/L for Co; and 250 μg/L for Pb. The accumulation of Cu, Ni and Co by Artemiu nauplii did not differ for animals exposed to single or combined heavy metal solutions. Cr, Zn and Pb had a synergistic effect of heavy metal uptake in combined heavy metal element solutions, however, Fe, Cd and Mn had an antagonistic effect.     

原子吸收法测定大嶝海域牡蛎中微量元素含量

采用火焰原子吸收光谱法对大嶝海域牡蛎鳃和肚腹中微量元素的含量进行测定,同时用加标回收法检验方法的可靠性。研究结果表明,牡蛎含有丰富的微量元素,鳃中Cu、Zn、Mn、Fe的含量分别为15.35±0.36μg/g、72.86±1.12μg/g、11.39±0.76μg/g、40.07±0.40μg/g;肚腹中Cu、Zn、Mn、Fe的含量分别为5.37±0.40μg/g、41.93±0.81μg/g、6.74±0.34μg/mg、24.89±0.53μg/mg。牡蛎鳃中Cu、Zn、Mn、Fe的含量均高于肚腹。用原子吸收方法测定牡蛎中微量元素的效果较好,回收率为89.0%～102.5之间,相对标准偏差在1.4%以下。     

花鳗、欧鳗和日本鳗肌肉无机元素的分析

采用电感耦合等等子体发射光谱仪对花鳗、欧鳗和日本鳗肌肉无机元素组成进行了测定。结果表明:花鳗肌肉中Ca含量最高,P含量次之。欧鳗和日本鳗肌肉中P含量最高,Ca含量次之。三种鳗鲡肌肉中Na、Mg、K含量相近且高低顺序相同,花鳗肌肉中常量元素和Zn、Fe、Mn的含量均高于欧鳗和日本鳗。三种鳗鲡肌肉中均含人体不可缺少的微量元素Zn。据此可认为花鳗营养价值最高。     

Use of biomass for the removal of heavy metals at low concentrations from freshwater for Chilean Atlantic salmon farms

In Chile and Norway, countries with the highest salmon production in the world, salmons have developed chronic diseases due to toxicity problems from free metallic ions. Aluminum (Al) and iron (Fe) were found to be present in freshwaters used by the Chilean salmon industry. In this work, different alternatives for Al and Fe removal were compared to achieve the required standards in salmon culture. Manganese (Mn) removal was also assessed since Fe and Mn removal can be accomplished in a single process.Since cellulose production (a principal economic activity in Chile) and the sawmill industry generate Pinus radiata bark as a waste product, this study also analyzed its application as an adsorbent of precipitate Al, Fe, and Mn in comparison with the traditional method of granular filtration. Al(OH)₃ precipitation was achieved by pH exchange. For precipitation of Fe and Mn oxides, two alternatives were analyzed: (i) oxidation by the presence of dissolved oxygen and pH exchange and (ii) pH exchange by CO₂ injection and oxidation produced by chemical filtration.Fe and Mn in solution, at low concentrations (less than 1 mg/L) presented a maximum precipitation at pH equal to 8.7, different from the value they presented individually. The separation efficiency of the three processes: (a) oxidation and filtration in column packed with P. radiata bark; (b) oxidation and granular filtration (smaller particle size); (c) CO₂ injection and chemical and granular filtration were of 93, 97 and 98%, for Fe and of 97, 99 and 29% for Mn, respectively. In all the studied alternatives, Fe concentrations less than 0.1 mg/L, compatible with salmon life, were obtained; in contrast for Mn, it was only possible to reach an adequate concentration for salmon life with the granular filter for smaller particle sizes.The optimum pH of Al precipitation was 6.4 and the column filled with P. radiata bark achieved Al concentration values less than 0.01 mg/L, limit value for salmon farms, obtaining removal efficiencies greater than 99.5%; in contrast, in the granular filter, the average obtained for cycle efficiency was 80.3%.Only the column filled with P. radiata bark achieves Al and Fe concentrations compatible with salmon life.     

Experimental insight of trace metal environmental pollution problems in mussel farming

A survey was made on the content of nine trace metals in waters of 12 predetermined coastal stations in the Island of Penang, Malaysia, with the object of establishing mussel culture farms in the near future. The results indicated low concentrations of these trace elements except for Cr and Ni, which ranged from trace level to 35 ppm and BDL (below detectable level) to 2.07 ppm, respectively. These values are slightly above the upper limits (Cr, 0.05 and Ni, 1.0 ppm) set by the national Division of Environment, Ministry of Science, Technology and Environment, under the Environmental Quality (Sewage and Industrial Effluents) Regulations 1978.Investigations on tissue level bioaccumulated trace metal contents in mussel from an experimental culture farm indicated BDL values for As in all tissues, Cd highest in the intestines and stomach (6.24 ppm), Co in the mantle (59.85 ppm), Cr in the siphon (1869.85 ppm), Cu in the mantle (23.94 ppm), Fe in the intestines and stomach (218.82 ppm), Mn in the style (365.28 ppm), Ni in the mantle (23.94 ppm), Pb in the mantle (279.3 ppm) and Zn in the style (152.2 ppm). However, culture experiments at 10 ppm concentration stresses of the different trace elements over a 48-h period did not result in a similar tendency in tissue bioconcentration, except for Cd (378.35 ppm) and Fe (419.66 ppm) in the intestine and stomach, and Mn (748.5 ppm) in the style. Co was highest in the style (187.35 ppm), Cr in the gill (2924.91 ppm), Cu in the gill (457.22 ppm), Ni in the intestines and stomach (222.44 ppm), Pb in the gill (1897.2 ppm), and Zn in the mantle (1077.73 ppm).Short-term stress studies over a 48-h period with trace metal concentrations ranging between 10 and 300 ppm indicated the patterns of biodeposition for Cd, Cr, Co, Pb, Mn and Zn to be closely related even though their toxicity levels varied. Cu indicated a bioaccumulation maximum after 12 h of incubation followed by a regulatory mechanism, while Fe and Ni demonstrated a drastic spiked absorption after 6 h exposure followed by the normal trend of biodeposition as observable for the other trace metals. The biodeposition factors at most instances, were highest for the 10 ppm concentration cultures of 48 h.     

Trace metal distribution in pelagic fish species from the north-west African coast (Morocco)

International Aquatic Research - In the current study, ten elements contents (Fe, Zn, Mn, Cu, Cr, Co, Ni, Cd, Pb and Hg) have been measured in muscle and liver of four pelagic fish species...     

长江水系3个湖泊中华绒蟹形态及元素“指纹”特征

以江苏省长江水系3个不同湖泊(太湖、石臼湖和固城湖)产中华绒螯蟹(Eriocheir sinensis)群体为研究对象,分别对其进行形态学和元素"指纹"特征的比较研究。基于16个组形态数据的框架测量及相应的逐步判别分析结果表明,虽然太湖、石臼湖和固城湖产中华绒螯蟹3群体之间在形态学上存在一定的差异,且判别准确率分别为70%、90%和80%,但其差异程度尚未达到能够有效区分3个群体的水平。统一使用中华绒螯蟹第三步足作为标准试样,应用电感耦合等离子质谱仪测定了其中21种元素的含量和分布特征,其中Cr、Co、As、Se、Cd、Pb、Tl、Ag、Mo、Ni未检出。与形态判别结果不同的是,3湖泊产中华绒螯蟹第三步足元素含量和分布的总体差异极为显著,太湖、石臼湖和固城湖产中华绒螯蟹的判别准确率分别高达100%、80%和100%。这表明本研究所尝试的中华绒螯蟹第三步足元素"指纹"分析判别方法具有有效区别不同产地中华绒螯蟹的潜力。     

Mineral composition of some commercial fish feeds available in Europe

The concentrations of 14 mineral elements (Na, K, Ca, P, Mg, Fe, Zn, Cu, Mn, Co, Cr, Ni, Cd and Pb), together with pH, moisture, ash and NaCl content, were determined in 38 feeds commonly available in Europe for trout (starter, fingerling, grower, brood), salmon (starter, fingerling, grower), eel (grower), and larval fishes.Large differences in the mineral composition, particularly the trace elements Fe, Zn, Cu, Mn, Co and Pb, exist within and between the different feed categories tested. The results obtained are discussed in the context of available information on the dietary mineral requirements of these fish species.