直接测汞仪测定食品中总汞

目的建立直接测汞仪测定食品中总汞的方法。方法采用直接测汞仪测定食品中的总汞,并对FAPAS 07322大豆粉样品采用直接测汞仪法、原子荧光光谱法、电感耦合等离子质谱法测定进行方法比对,结合FAPAS 07322能力验证报告对直接测汞仪法进行评价。结果直接测汞法在低浓度范围(0～20 ng)和高浓度范围(20～300ng)的相关系数均能达到0.999,方法检出限为0.07μg/kg,精密度小于8.0%,回收率范围为90.0%～103.5%。FAPAS 07322测定结果为323μg/kg, Z值为0.0,接近实验室比对中位值。结论直接测汞仪测定食品中的总汞,操作简便快捷,结果准确,适用于食品中总汞的分析。     

保健食品中总汞测定方法的比较

摘要：目的 验证测汞仪直接固体进样测定保健食品中总汞的结果可靠性。方法 采用测汞仪固体直接进样和原子荧光光谱法两种方法对保健食品中的总汞进行测定。结果 几种不同浓度加标的保健食品测汞仪测定的总汞结果与原子荧光法测定结果相符,回收率在88%～116%之间、RSD<10%。结论 测汞仪直接固体进样测定保健食品中总汞的方法具有准确、快捷、运行成本低、无环境污染等优点,和现有国标原子荧光法测定同一样品,测定结果具有可比性,方法具有可推广性。     

测汞仪法测定植物油中微量汞的研究

建立测汞仪法测定植物油中微量汞的新方法。将植物油样品直接称量于石英舟中,在样品分解炉中干燥,载气高纯氧气中充分燃烧释放出汞,经催化还原成原子化态汞,与金膜富集形成金汞齐,在850 ℃快速加热释放出汞,在汞特征波长253.6 nm下测定汞的含量。方法检出限为0.2 μg/kg,相对标准偏差为1.3%～3.6%(n=6),加标回收率为92.8%～96.9%。该方法快速、稳定,重现性良好,适用于植物油中微量汞的快速测定。     

电热解—塞曼原子吸收光谱法用于总膳食样品中痕量汞的快速测定

目的进一步推进测汞仪在低含量样品总汞含量检测中的运用。方法将标准加入法技术运用到直接测汞仪测定样品总汞含量中,测定部分总膳食样品。同时,采用食品安全国家标准中的原子荧光光谱法对同种样品的总汞含量再次测定。结果运用原子荧光光谱法对低汞含量总膳食样品进行检测,样品总汞含量范围为1.33~41.14μg/kg;运用测汞仪标准加入法对低汞含量总膳食样品进行检测,样品总汞含量范围为1.32~32.07μg/kg。测汞仪标准加入法与原子荧光光谱法对同种总膳食样品中总汞含量检测结果接近。结论引入标准加入法技术的测汞仪方法不仅具有省时、快速检测的优势,而且可以保证测定结果的准确性。     

超级微波消解-电感耦合等离子体质谱法与测汞仪法测定茶叶中总汞含量的比较

目的比较超级微波消解-电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry,ICP-MS)和测汞仪法测定茶叶中总汞(Hg)的含量情况。方法第一法采用超级微波进行消解, ICP-MS检测,外标法定量。第二法为测汞仪法,无需消解前处理,采用直接进样方式,外标法定量。结果在最优仪器条件下,超级微波消解-ICP-MS法测定的Hg在0～2 ng/mL范围内线性关系良好,相关系数为1.0000,方法检出限为1μg/kg。方法成功用于40个茶叶样品(包括红茶、绿茶、白茶、黄茶、花茶、乌龙茶、袋泡茶、紧压茶和黑茶)中Hg的测定,样品加标回收率在95.5%～106.4%之间,相对标准偏差(relative standard deviation,RSD)均不超过3.86%。测汞仪法测定Hg在0～20 ng范围内线性关系良好,相关系数为0.9997,方法检出限为0.05μg/kg。测汞仪法同样用于40个茶叶中Hg的测定,样品加标回收率在93.2%～103.7%之间,RSD不超过6.65%。结论两种测定方法简便快速、准确、灵敏度高,均能为快速测定茶叶中总汞元素提供有效的分析方法。测汞仪法相对波动较大,但是能满足检验检测需求。     

电感耦合等离子体质谱法与直接测汞仪法测定食品级润滑油中汞含量的比较

本文比较电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry, ICP-MS)和直接测汞仪法测定食品级润滑油中总汞(Hg)的含量情况。第一法微波进行消解-ICP-MS 检测,内标法定量。在最优仪器条件下,微波消解-ICP-MS法测定的Hg 在0.5~20μg·L-1范围内线性关系良好,相关系数为0.9998, 方法检出限为0.5μg/kg。重复性测试（n=10）,相对标准偏差(relative standard deviation, RSD) 为4.15%,样品加标回收率(n=7) 在95.21%—104.57%之间;第二法为测汞仪法,无需消解前处理,采用直接进样方式, 外标法定量。测汞仪法测定 Hg 在5.00~200μg·L-1范围内线性关系良好, 相关系数为0.9997,方法检出限为0.5μg/kg 。方法重复性测试（n=10）,相对标准偏差为3.42%,样品加标回收率 (n=7) 在94.87%-98.40%之间。两种测定方法准确、灵敏度高,均能测定食品级润滑油中总汞元素。ICP-MS需经微波消解,样品前处理较为复杂,直接测汞仪可以不经前处理直接进样,操作较为简单方便。各实验室可根据自身条件选择合适的方法开展测定食品级润滑油中总汞元素的含量,考虑到仪器的承载量和检测时间周期,如为大量检测可选择微波消解-ICP-MS检测法;如果少量检测可选择直接测汞仪法,操作简单方便。     

测汞仪固体直接进样测定保健食品中总汞的方法研究及方法比较

目的 研究测汞仪固体直接进样方法测定保健食品中总汞,通过与国标方法比较验证结果的可靠性.方法 采用测汞仪固体直接进样和原子荧光光谱法两种方法对保健食品中的总汞进行测定.结果 几种不同浓度加标的保健食品测汞仪测定的总汞结果与原子荧光法测定结果相符,回收率在88％～116％之间,RSD＜ 10％.结论 测汞仪直接固体进样测定保健食品中总汞的方法具有准确、快捷、运行成本低、无环境污染等优点,和现有国标原子荧光法测定同一样品,测定结果具有可比性,方法具有可推广性.     

直接测汞仪测定茶叶中的汞

本文建立了全自动直接测汞仪测定茶叶中汞的方法。样品经粉碎混匀后,无需任何其他前处理,即可采用全自动直接测汞仪进行测定,外标法定量。本法线性范围为0～5 ng(汞的质量),方法检出限为0.01 ng。直接测汞仪法6次测定两种茶叶标准物质中汞含量值的相对标准偏差分别为4.0%和4.2%。     

直接进样测汞法测定乳粉、干香菇中总汞含量

目的是建立直接测汞仪测定乳粉、干香菇中的总汞含量分析方法——直接进样测汞法。实验结果如下：线性回归方程：y=0.05360176x-0.00093549线性范围：0-20ng相关系数：R²=0.9999检出限：0.056μg/kg加标回收率：93.7%-103.3%。通过分析测定，该方法操作步骤简便、结果快速、准确、灵敏度高，是一种食品中总汞含量测定的快速准确方法。     

测汞仪快速测定保健食品中的总汞含量

建立了一种固、液体食品中总汞含量快速检测方法。通过测汞仪内置的模块化干燥、热分解、催化还原、金汞齐化、冷原子吸收等组件对样品中汞进行一站式的检测,无需对样品进行传统的前处理,避免了样品中汞的污染与损失。该法根据汞浓度建立了高、低两条浓度范围(0~20 ng和20~800 ng)的标准曲线,具有检出范围宽(0~800 ng)、检出限低(LOD=0.06μg/kg)等特点。采用该法测定了固、液态等6种保健食品中总汞的含量,并与现行的食品中总汞的测定国家标准方法进行了比较,两种方法的检测结果无显著性差异,通过对标准物质的测定验证表明该法测定结果准确可靠。高、中、低三个浓度水平回收实验测得回收率为93.20~106.00%,回收结果令人满意。该方法可推荐作为食品、农产品等国家食品安全抽检工作的快速检测方法。     

新疆昌吉地区食用菌中汞和镉含量的分析检测

目的了解昌吉地区食用菌中重金属汞和镉含量的情况,保障食用菌安全性。方法在昌吉地区的超市、农贸市场等地随机采集7种不同的食用菌,依据国标(GB5009.17食品中汞的检测第一法;GB5009.15食品中镉的检测第一法)测定其中汞和镉的含量,同时采用单因子污染指数法和综合因子污染指数法对食用菌的污染程度进行评价。结果 210种样品中汞超标率0.95%,镉超标率2.38%,且同种食用菌对不同重金属的富集能力有差异,黑平菇、鸡腿菇、平菇、金针菇、圆菇和杏鲍菇的富集趋势均为镉总汞;而香菇的富集趋势则为总汞镉。分级结果为金针菇、黑平菇、鸡腿菇、平菇、杏鲍菇为一级产品;圆菇为二级产品;香菇为三级产品。不同采样点中汞污染最高的是源自农贸市场的食用菌,平均值为0.054 mg/kg;镉污染最高的是市场,平均值为0.059 mg/kg。结论昌吉大部分地区重金属污染较为严重,可能是食用菌生长环境中重金属含量较高所致,因此需要从栽培源头加大控制防范力度。     

测汞仪/高效液相色谱-电感耦合等离子体质谱联 用法测定鱼松中总汞和甲基汞的含量

目的测汞仪和高效液相色谱-电感耦合等离子体质谱法(high performance liquid chromatography-inductively coupled plasma mass spectrometry,HPLC-ICP-MS)测定鱼松中总汞及甲基汞的含量。方法样品粉碎均匀后,无需前处理环节,直接通过测汞仪内置的模块对样品中的总汞进行一站式检测。以L-半胱氨酸-乙酸铵-甲醇-盐酸为提取液,高效液相色谱分离,ICP-MS为检测手段对样品中的甲基汞进行测定。结果在优化的检测条件下,总汞的检出限为0.05μg/kg,甲基汞的检出限为0.001 mg/kg;5种鱼松样品中总汞的加标回收率为80.2%~109.6%,甲基汞的回收率为85.0%~108.5%,样品中总汞和甲基汞的相对标准偏差均小于8.0%。样品中甲基汞在总汞中的含量约为49.3%~82.5%,是汞的主要存在形态。结论该方法操作简便、提取效率高,可实现鱼松样品中总汞和甲基汞的快速测定。     

Mercury in fruiting bodies of dark honey fungus (Armillaria solidipes) and beneath substratum soils collected from spatially distant areas

BACKGROUND: This paper reports data on bioconcentration potential and baseline mercury concentrations of fruiting bodies of dark honey fungus (Armillaria solidipes) Peck and soil substrate layer (0–10 cm) from 12 spatially distant sites across Poland. Mercury content of caps, stipes and soil samples were determined using validated analytical procedure including cold‐vapor atomic absorption spectroscopy after thermal decomposition of the sample matrix and further amalgamation and desorption of mercury from gold wool. RESULTS: Mean mercury concentrations ranged from 20 ± 8 to 300 ± 70 ng g^?1 dry weight (dw) in caps, from 20 ± 6 to 160 ± 40 ng g^?1 dw in stipes, and in underlying soil were from 20 ± 2 to 100 ± 130 ng g^?1 dw. The results showed that stipes mercury concentrations were 1.1‐ to 1.7‐fold lower than those of caps. All caps and the majority of stipes were characterized by bioconcentration factor values > 1, indicating that dark honey fungus can be characterized as a moderate mercury accumulator. CONCLUSION: Occasional or relatively frequent eating of meals including caps of dark honey fungus is considered safe in view of the low total mercury content, and the mercury intake rates are below the current reference dose and provisionally tolerable weekly intake limits for this hazardous metal. © 2012 Society of Chemical Industry     

高效液相色谱-电感耦合等离子体质谱法测定鱼肉中甲基汞、乙基汞含量的不确定度评定

目的 评定采用高效液相色谱-电感耦合等离子体质谱(High performance liquid chromatography combined with inductively coupled plasma-mass spectrometry, HPLC-ICP-MS)法检测鱼肉中甲基汞、乙基汞含量的不确定度。方法 分析整个检测过程中存在的不确定度因素,建立数学模型,分别从称样量、稀释体积、标准溶液、标准曲线拟合以及方法回收率等几个方面进行分析,对测量结果的不确定度进行评定。结果 影响测量结果的不确定度主要来源于样品前处理和标准曲线拟合。鱼肉样品中结果表示分别为：甲基汞含量（0.48±0.046） mg/kg;乙基汞含量为（0.34±0.051） mg/kg, k=2。结论 该方法准确度高,适用于鱼肉中甲基汞、乙基汞的检测,为提高数据准确性提供有效指导。     

干巴菌中部分重金属元素及无机砷、 甲基汞含量分析

目的检测干巴菌中5种重金属总砷、总汞、铅、镉、铬及无机砷和甲基汞的含量,探讨干巴菌对重金属的生物富集作用。方法采用电感耦合等离子体质谱法检测总砷、总汞、铅、镉含量,采用液相原子荧光光度计联用检测无机砷、甲基汞的含量。结果 31份干巴菌样品中总砷、总汞、铅、镉的检出率均为100%,无机砷的检出率为50%,甲基汞在全部样品中均未检出。昆明的干巴菌样品中砷含量较高,达0.46 mg/kg;曲靖的干巴菌中铅含量有0.9997 mg/kg;镉含量较高,为0.46 mg/kg。结论总体来看不同地区的干巴菌中总砷、总汞、镉、铬、无机砷和甲基汞的含量处于较低水平,但铅含量偏高。干巴菌对重金属没有特异性吸收富集能力。     

预富集-冷原子吸收光谱法测定水中的痕量汞

建立了一种预富集-冷原子吸收光谱法测定水中的痕量汞的方法,研究了预富集条件、测定条件等对灵敏度的影响.在最佳的条件下,用这个方法测定水样中的痕量汞,150ml样品中,特征质量为0.01ng/1%,标准偏差为0.0008～0.001,回收率为95.0%～100.0%,结果较为满意.     

Determination of mercury in fish by cold vapour atomic absorption spectrometry using an automatic mercury analyzer

The concentration of mercury in fish samples from the Atlantic coast of Ghana was determined using a simple, rapid and accurate method. A mixture of HNO₃, HClO₄ and H₂SO₄ was used for complete oxidation of organic tissue. Mercury is detected by the cold vapour atomic absorption spectrometry technique using an automatic mercury analyzer developed at the National Institute for Minamata Disease (NIMD). In total, 56 samples covering 13 species of fish were analysed for total mercury. The concentration of mercury in the edible muscle tissue of these fish ranged from 0.004 to 0.122 μg g⁻¹ wet weight. All fish species sampled had concentrations less than the WHO limit of 0.5 μg g⁻¹ wet weight. The low concentrations of mercury detected in the samples do not constitute any significant mercury exposure to the general population through fish consumption.     

Method development for the control determination of mercury in seafood by solid-sampling thermal decomposition amalgamation atomic absorption spectrometry (TDA AAS)

A very simple and rapid method for the determination of total mercury in fish samples using the Direct Mercury Analyser DMA-80 was developed. In this system, a previously weighted portion of fresh fish is combusted and the released mercury is selectively trapped in a gold amalgamator. Upon heating, mercury is desorbed from the amalgamator, an atomic absorption measurement is performed and the mercury concentration is calculated. Some experimental parameters have been studied and optimised. In this study the sample mass was about 100.0 mg. The relative standard deviation was lower than 8.0% for all measurements of solid samples. Two calibration curves against aqueous standard solutions were prepared through the low linear range from 2.5 to 20.0 ng of Hg, and the high linear range from 25.0 to 200.0 ng of Hg, for which a correlation coefficient better than 0.997 was achieved, as well as a normal distribution of the residuals. Mercury reference solutions were prepared in 5.0% v/v nitric acid medium. Lyophilised fish tissues were also analysed; however, the additional procedure had no advantage over the direct analysis of the fresh fish, and additionally increased the total analytical process time. A fish tissue reference material, IAEA-407, was analysed and the mercury concentration was in agreement with the certified value, according to the t-test at a 95% confidence level. The limit of quantification (LOQ), based on a mercury-free sample, was 3.0 μg kg(-1). This LOQ is in accordance with performance criteria required by the Commission Regulation No. 333/2007. Simplicity and high efficiency, without the need for any sample preparation procedure, are some of the qualities of the proposed method.     

Analytical procedure for total mercury determination in fishes and shrimps by chronopotentiometric stripping analysis at gold film electrodes after microwave digestion

A method for the total mercury determination in fish and shrimps employing chronopotentiometric stripping analysis on gold film electrodes is described. Fish and shrimp tissues were digested using a microwave oven equipped with closed vessels. We developed a microwave heating program which decomposed all the samples employing diluted nitric acid and hydrogen peroxide. The proposed method was validated by analyzing a certified reference material and then applied for different fish species from fresh water and seawater acquired in local markets of São Paulo city, Brazil. The Brazilian legislation establishes 0.5 and 1 mg per kilogram of fish as upper limit of mercury for omnivorous and predator species, respectively. Except for blue shark tissues, the mercury content was situated below 0.5 μg g⁻¹ for all the analyzed samples. The detection limit of the proposed method was calculated as 5 ng g⁻¹ of sample utilizing 5 minutes of electrodeposition (+300 mV vs. Ag/AgCl) on the gold electrode.     

高效液相色谱-原子荧光光谱法测定水产品中 不同形态汞含量

目的建立高效液相色谱-原子荧光光谱法(high efficiency liquid chromatography-atomic fluorescence spectroscopy,HPLC-AFS)测定水产品中不同形态汞的含量,并以高效液相色谱-电感耦合等离子体质谱法(high efficiency liquid chromatography-inductively coupled plasma-mass spectrometry,HPLC-ICP-MS)进行方法确证。方法样品中的汞元素经5 mol/L HCl溶液提取,用6 mol/L Na OH溶液中和样品,L-半胱氨酸作为流动相中的汞配位剂,用于样品中不同形态汞的分离。结果汞化合物在质量浓度为1.0~20.0μg/L范围内,浓度和光谱峰面积间呈良好的线性关系。方法检出限分别为:无机汞0.009 mg/kg、甲基汞0.006 mg/kg和乙基汞0.009 mg/kg;加标回收率为81.0%~117.0%,相对标准偏差为3.59%~7.30%。用本方法对FAPAS质控样品蟹肉罐头T07231QC中的甲基汞进行测定,测定的结果值与参考值相符。结论该方法操作简单、灵敏度高、重现性好,适用于水产品中不同形态汞含量的测定及结果确证。