ICP-MS测定饼干中的铅、砷、铬、镉、铜、锌、铁和锰

探讨了应用电感耦合等离子体质谱仪测定饼干中铅、砷、铬、镉、铜、锌、铁和锰8种重金属元素的方法。运用微波消解系统对样品进行消解,以铋、锗、钪和铟作为内标物,用ICP-MS对消解液进行检测,并采用国标方法对其结果进行验证。利用加标回收率试验和国家标准物质小麦(GBW 10052)检测试验考察了方法的准确性和可靠性。结果表明,该方法所测元素在标准溶液浓度范围内呈线性关系,相关系数均大于0.999,方法检出限在0.002~0.500 mg/kg之间,相对标准偏差均小于6.55%,本法与国标方法测量结果的相对偏差在3.73%~8.40%之间,加标回收率在88.0%~106%之间,标准物质的测定值与标准参考值符合要求。     

ICP-MS测定食品模拟物中的铅、砷、镉、镍、钴、锌

建立了电感耦合等离子质谱(ICP-MS)测定食品模拟物中铅、砷、镉、镍、钴、锌的方法。分别用水、3%(V/V)乙酸水溶液、10%(V/V)乙醇水溶液、95%(V/V)乙醇水溶液在40℃下浸泡涂有内涂层的金属饮料罐两片罐和三片罐240 h,得到食品模拟物样品。对于水、3%(V/V)乙酸水溶液、10%(V/V)乙醇水溶液三种食品模拟物样品,用电热板将样品蒸发至近干,用10%硝酸定容,上机检测。对于95%(V/V)乙醇模拟物样品,用电热板将样品蒸发至近干,剩余液体过滤后用10%(V/V)硝酸定容,上机测试。方法的检出限在0.5 ng/mL到15 ng/mL之间,线性良好,相关系数均≥0.999;在两个浓度水平进行添加实验,大部分回收率在92.3%~108%之间,相对标准偏差在0.3%～13.3%之间。方法准确度高,操作简单,是检测食品模拟物中铅、砷、镉、镍、钴、锌的有效方法。     

A simplified method for the extraction of the metals Fe,Zn, Cu,Ni, Cd,Pb, Cr,Co and Mn from soils and sewage sludges

The method described for digestion of soil samples with aqua regia is simple, flexible and safe to operate with large sample throughout. At least nine metals can be determined in the resulting solutions with errors of <5%. The results compare favourably with those from reflux aqua regia and averaged 88% of the certified total values for reference soils and 88% of those for reference sewage sludges.     

Influence of olive cultivars and period of harvest on the contents of Cu,Cd, Pb,and Zn in virgin olive oils

Levels of four of the major pollutant heavy metals were assessed by ICP-OES in virgin olive oil monocultivar samples. The data showed high variability within cultivars for lead and zinc, whereas, for cadmium and copper, no statistical difference was observed. The influence of the cultivar and the stage of ripening of olives on heavy metal content was assessed; zinc was the only metal with a great variability within the first and the second harvest. All olive samples were processed with the same milling apparatus.     

The effect of storage of canned vegetables on concentration of the metals Fe, Cu, Zn, Pb, Sn, Al, Cd and Ni

The increase in the concentration of Fe, Cu, Zn, Pb, Sn, Al, Cd and Ni over a 2 year's time of strongly corrosive acidic vegetables (pickles) and weakly corrosive vegetables (peas, green beans, haricot beans, mushrooms) has been determined. The results show a considerable increase in Fe, Cu, Pb and Sn content with time, particularly for pickles, while the change in Al, Cd, Zn and Ni content was rather negligible.     

The effect of storage of canned meat on concentration of the metals Fe, Cu, Zn, Pb, Sn, Al, Cd and Ni

Storage of canned foods may enrich the concentration of some metals. Because their toxic and other properties the presence of which in foods over certain limits is undesirable. Therefore we have determined the contents of Fe, Cu, Zn, Pb, Sn, Al, Cd and Ni over a 2 years' time of bovine, pork and veal meat. The results show a gradual increase in the concentration of Fe, Cu, Sn and Zn with time in the order pork greater than bovine greater than veal.     

ICP-MS法同时测定卷烟滤嘴用丝束中的铬、镍、铜、砷和铅

采用HNO3/H2O2微波4步消解-电感耦合等离子体质谱法同时测定了醋酸纤维和聚丙烯纤维丝束中Cr、Ni、Cu、As、Se、Cd和Pb元素,并对第4步消解时间进行了优化。结果显示:①第4步消解的适宜条件为190℃下消解20min;②各元素的回收率在86.38%～117.2%之间,RSD<25%,检出限25.20～245.1ng/L;③2种丝束样品中均未检出Se和Cd。     

ICP-MS法同时测定烟草中的铬、镍、砷、硒、镉、汞、铅

采用微波消解和电感耦合等离子体质谱法同时测定了85个烟叶样品中的铬(Cr)、镍(Ni)、砷(As)、硒(Se)、镉(Cd)、汞(Hg)和铅(Pb)含量。结果表明:①这些重金属元素的回收率96.34%~106.7%,检出限7.974~147.8ng/L,相对标准偏差1.41%~9.78%;②烟叶中的Cr、Ni、As、Se、Cd、Hg和Pb含量随品种和产地的不同差别较大,同一品种不同部位烟叶的差别相对较小。     

Determination of Zn,Cu, Cd,Pb, Ni and Cr in some Slovenian foodstuffs

An acid-assisted microwave digestion procedure was optimised for the determination of trace elements in foodstuffs by the use of flame and electrothermal atomic absorption spectrometric (FAAS, ETAAS) techniques. Zn, Cu, Cd, Pb, Ni and Cr were determined in cabbage, wheat, potato, instant milk, fish, eggs and baby foodstuffs. The repeatability of measurements was tested in the cabbage sample and was found to be ±3.3% for Zn, 4.6% for Cd, ±6.8% for Cu and ±15.5% for Cr. The worse value obtained for Cr was probably due to its inhomogeneous distribution and very low concentration in the cabbage. Concentrations of Ni and Pb in the cabbage sample were below the limit of detection (0.2 mg kg^–1). The accuracy of the analytical procedure was checked by the analysis of the standard reference material CRM 1570 Trace and minor elements in spinach leaves and IAEA 336 Trace and minor elements in lichen. Good agreement between the certified or indicative and determined values was obtained. The results indicate that the concentrations of Zn, Cu, Cd, Pb, Ni and Cr found in cabbage, wheat and potato are comparable to the literature data. Cd, Pb and Ni were not found to be the contaminants in the foodstuffs analysed. Higher concentrations of Ni were found only in baby food "okolenik", arising from the cocoa that "okolenik" contained. It was demonstrated that the Cr content is very low in baby food, yolk and white of egg and in fish (<0.05 mg kg^–1 Cr). Elevated concentrations of trace elements were found only in mussels that accumulate heavy metals from the marine environment.     

The effect of storage of canned juices on content of the metals Fe, Cu, Zn, Pb, Sn, Al, Cd, Sb and Ni

The increase in concentration of iron, copper, zinc, lead, antimony, aluminium, cadmium, tin and nickel over a 2 year's time of juices of peach (prunus persica), pear (pyrus communis), apricot (prunus vulgaris) and apple (malus pumila) was determined. The results show a considerable increase in Fe, Cu, Pb, Zn and Sn with time, while the change in Al, Cd, Ni and Sb is negligible.     

Estimation of uncertainties of the method to determine the concentrations of Cd, Cu, Fe, Pb, Sn and Zn in tomato paste samples analysed by high resolution ICP-MS

Cadmium, copper, iron, lead, tin and zinc were determined in tomato paste samples by using high resolution inductively coupled plasma mass spectrometry. This study was a part of Proficiency Testing scheme conducted by National Metrology Institute (UME) of Turkey. The method was validated. The percentage relative errors obtained for each element ranged between 1.4% and 9.0% for NIST SRM 1573a, tomato leaves. Measurement uncertainties of all elements were calculated by applying bottom-up approach. The calculated percentage relative uncertainties for the elements were between 8.2% and 16.4%. The major contributions to the uncertainty budget came from the calibration curves, repeatability and recovery. Tomato paste samples gathered from the supermarkets in Turkey were analysed by using the validated method. Their levels were compared both with the literature values and European Commission Regulations.     

稀酸提取-ICP-MS法快速测定大米中锰、铜、锌、铅、镉、铷、锶含量的研究

本文建立了常温条件下,利用稀酸提取-电感耦合等离子体质谱法快速测定大米中元素(锰、铜、锌、铅、镉、铷、锶)的方法。实验通过优化影响提取的各个因素,确定了最终提取条件。该方法各元素的回收率均在90%~111%,且标准物质相关元素的浸提结果均在相应赋值范围内。多家实验室联合验证的统计结果显示7家实验室的各元素HorRat值均小于1,表明该方法拥有很好的重现性和再现性。稀酸温和提取-电感耦合等离子体质谱法具有高效、快速、准确的特点,可将样品处理时间缩短至30 min内,与经典微波消解-ICP-MS法比较,锰、铜、锌、铅、镉、铷、锶元素的测定值无显著性差异(p>0.05)。     

Determination of Cd,Co, Cu,Fe, Pb,Mn, Ni and Zn in diets: Development of a method

A method useful for the determination of cadmium, cobalt, copper, iron, lead, manganese, nickel and zinc in diets is described. Organic matter is destroyed applying a wet procedure, and element content is measured by flame atomic absorption spectroscopy (FAAS) in the case of copper, iron, manganese, nickel and zinc, and by graphite furnace (GF-AAS) in the case of cadmium, cobalt and lead. The matrix interference study is carried out. Values found for linearity, detection and quantitation limits as well as accuracy show that the described method is useful to determine the elements taken into account at usual levels in diets.     

The levels of heavy metals (Mn, Fe, Co, Ni, Cu, Zn, Cd, Pb, Hg) in fish from onshore and offshore waters of the German Bight

Zusammenfassung Mit dem Ziele, unsere Kenntnisse über den gegenwärtigen Grad der Schwermetallspeicherung in Fischen zu erweitern, wurde der Gehalt an den metallischen Spurenelementen Mangan, Eisen, Kobalt, Nickel, Kupfer, Zink, Cadmium, Blei und Quecksilber in bestimmten Fischarten (Kabeljau und Scholle) aus küstennahen und küstenfernen Fanggebieten der Deutschen Bucht bestimmt. Als Meßverfahren wurde die Atom-Absorptions-Spektrophotometrie eingesetzt: Bei der Bestimmung der Elemente Mn, Fe, Cu und Zn wurde die herkömmliche Flammentechnik (Laminarbrenner, Luft-Acetylen-Flamme) verwendet. Die flammenlose Atom-Absorptions-Spektrophotometrie unter Verwendung der Graphitrohrküvette diente der Bestimmung von Cd, Pb, Co und Ni. Der Gehalt an Gesamt-Quecksilber wurde mit der sogenannten Kaltdampf-Methode ermittelt. Zur Vermeidung von Fehlinterpretationen der Meßwerte von Kobalt und Nickel, die sich insbesondere bei diesen Elementen als Folge von Matrixeffekten ergeben, wurde eine spezielle Aufarbeitungstechnik entwickelt, die auf einer selektiven Abtrennung und Anreicherung durch Chelataustauscher-Chromatographie über Chelex 100 beruht.Die ermittelten analytischen Daten werden in einem Diagramm mit doppelt logarithmischem Maßstab dargestellt. Auf der Abscisse ist der Gehalt (Mittelwert von Mehrfachbestimmungen) aufgetragen, auf der Ordinate die zugehörige Reproduzierbarkeit (als Variationskoeffizient) des jeweiligen Meßverfahrens. Allen untersuchten Elementen lassen sich gut umrissene Gehaltsbereiche zuordnen.Das Spektrum der Gehalte an den Übergangsmetallen Mangan, Eisen, Kobalt, Nickel, Kupfer und Zink zeigt bei einem Vergleich von Fischen gleicher Art, aber verschiedener Herkunft nur geringe Unterschiede. Ebenso entsprechen einander die Gehalte, welche an Hand der Untersuchungen verschiedener Fischarten (Kabeljau, Scholle) gleicher Herkunft gewonnen wurden. Die ermittelten Werte für Cadmium, Blei und Quecksilber lassen erkennen, daß Schollen, die sich in der unmittelbaren Küstenzone aufhalten, erhöhte Gehalte aufweisen.

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The levels of heavy metals (Mn, Fe, Co, Ni, Cu, Zn, Cd, Pb, Hg) in fish from onshore and offshore waters of the German Bight

Summary With the intention of increasing our knowledge about the actual degree of heavy metal accumulation in fish, the contents of the elements manganese, iron, cobalt, nickel, copper, zinc, cadmium, lead and mercury in certain fish species (cod and plaice) from onshore and offshore waters of the German Bight have been determined. The measurements have been performed by atomic absorption spectrophotometry: Flame AAS was used as investigating procedure for the determination of Mn, Fe, Cu and Zn. A non-flame atomization system with a heated graphite tube was used for the determination of Cd, Pb, Co, and Ni. The concentration of total Hg was estimated according to the so-called cold vapour atomic absorption method. In order to avoid errors in interpretation of measured values of Co and Ni, which occured as a result of matrix effects, a special technique has been developed. This based upon an selective separation and enrichment by chelate exchanger chromatography (Chelex 100).The analytical data obtained are plotted in a diagram with log.-log. scale. The content is shown on thex-axis, and the corresponding relative reproducibility (variation coefficient) of the method used is shown on the y-axis. For all elements investigated certain levels have been found out.From an examination of the results it appeared that there were comparatively small differences in the prevailing concentrations of transition metals Mn, Fe, Co, Ni, Cu, and Zn between samples of the same species from different areas. Likewise, the levels estimated for plaice did not differ from those estimated for cod. There is some evidence of elevated levels of Cd, Pb, and Hg in plaice from areas along the coastline.

     

Li, Cr, Mn, Co, Ni, Cu, Zn, Se and Mo levels in foodstuffs from the Second French TDS

In 2006, the French Food Safety Agency (AFSSA) conducted the Second French Total Diet Study (TDS) to estimate dietary exposures to the main minerals and trace elements from 1319 samples of foods typically consumed by the French population. The foodstuffs were analysed by inductively coupled plasma-mass spectrometry (ICP-MS) after microwave-assisted digestion. Occurrence data for lithium, chromium, manganese, cobalt, nickel, copper, zinc, selenium and molybdenum were reported and compared with results from the previous French TDS. The results indicate that the food groups presenting the highest levels of these essential trace elements were “tofu” (for Li, Mn, Ni, Cu, Zn and Mo),“fish and fish products” particularly “shellfish” (for Li, Co, Cu, Zn, Se and Mo), “sweeteners, honey and confectionery” particularly dark chocolate (for Cr, Mn, Co, Ni and Cu), “cereals and cereal products” (for Mn, Ni and Mo) and “ice cream” (for Cr, Co and Ni).     

Fast Determination of Cd, Fe, Pb, and Zn in Food using AAS

Analytical chemistry plays a fundamental role in proposing fast and reliable procedures to analyze food samples. Proper selection and introduction of complementary foods during the breastfeeding period and childhood reduce the vulnerability to micronutrient deficiencies. This study aimed to propose a sensitive approach for the promotion of adequate food supplements regarding Cd, Fe, Pb, and Zn content. These metals were determined using flame atomic absorption spectrometry (Fe and Zn) and thermospray flame furnace atomic absorption spectrometry (Cd and Pb). A simple procedure mixing the sample (100 mg) with 0.1 mol/L HCl was proposed. Cadmium and Zn showed suitable results when a bovine liver certified sample (SRM 1577b) was studied, and the Fe content was strongly correlated to the size of the particle. Cadmium and Pb were not found in the food samples studied.     

The levels of heavy metals (Mn, Fe, Co, Ni, Cu, Zn, Cd, Pb, Hg) in fish from onshore and offshore waters of the German bight.

With the intention of increasing our knowledge about the actual degree of heavy metal accumulation in fish, the contents of the elements manganese, iron, cobalt, nickel, copper, zinc, cadmium, lead and mercury in certain fish species (cod and plaice) from onshore and offshore waters of the German Bight have been determined. The measurements have been performed by atomic absorption spectrophotometry: Flame AAS was used as investigating procedure for the determination of Mn, Fe, Cu and Zn. A non-flame atomization system with a heated graphite tube was used for the determination of Cd, Pb, Co, and Ni. The concentration of total Hg was estimated according to the so-called "cold vapour atomic absorption method". In order to avoid errors in interpretation of measured values of Co and Ni, which occured as a result of matrix effects, a special technique has been developed. This based upon an selective separation and enrichment by chelate exchanger chromatography ("Chelex 100"). The analytical data obtained are plotted in a diagram with log.-log. scale. The content is shown on the x-axis, and the corresponding relative reproducibility (variation coefficient) of the method used is shown on the y-axis. For all elements investigated certain levels have been found out. From an examination of the results it appeared that there were comparatively small differences in the prevailing concentrations of transition metals Mn, Fe, Co, Ni, Cu, and Zn between samples of the same species from different areas. Likewise, the levels estimated for plaice did not differ from those estimated for cod. There is some evidence of elevated levels of Cd, Pb, and Hg in plaice from areas along the coastline.     

Determination of Cd, Co, Cu, Fe, Pb, Mn, Ni and Zn in diets: development of a method.

A method useful for the determination of cadmium, cobalt, copper, iron, lead, manganese, nickel and zinc in diets is described. Organic matter is destroyed applying a wet procedure, and element content is measured by flame atomic absorption spectroscopy (FAAS) in the case of copper, iron, manganese, nickel and zinc, and by graphite furnace (GF-AAS) in the case of cadmium, cobalt and lead. The matrix interference study is carried out. Values found for linearity, detection and quantitation limits as well as accuracy show that the described method is useful to determine the elements taken into account at usual levels in diets.     

ICP-MS与GF-AAS测定饮用水中镍、铬、镉、铅含量的对比分析

电感耦合等离子质谱法(inductively coupled plasma massspectrometry,ICP-MS)与石墨炉原子吸收光谱法(graphite furnace atomic absorptionspectrometry,GF-AAS)是灵敏度较高的两种检验水中重金属含量的方法。本试验采用两种方法对天然饮用水,自来水、矿泉水、白开水、纯净水中水样品中铅、镉、铬、镍的检出限、精密度和加标回收率等数据进行对比分析,结果发现在检测杂质较多的水样时相对标准偏差较高,准确度也会相应的下降,石墨炉原子吸收光谱法影响较为严重。电感耦合等离子质谱法样品制备简单、检测过程干扰因素较少、检测过程方便,一次进样就可以得到多种元素的检测结果,检测速度远快于石墨炉原子吸收光谱法。电感耦合等离子质谱法优于石墨炉原子吸收光谱法,且各元素的检测结果稳定,精密度和加标回收率波动小,满足现代社会大批量检测的需求,检测准确性高,更适合检测重金属元素。     

微波消解-火焰原子吸收光谱法测定百里香中微量元素

采用微波消解-火焰原子吸收光谱法(FAAS法),连续测定雷山县乌东村的百里香中的Zn,Fe,Cu,Mn,Ni,Cd,Cr,Pb含量。待测元素的最佳测试条件经过正交试验设计优化组合确定。结果表明,供试样品中微量元素Zn,Fe,Cu,Mn的含量分别为154.6,331.4,1.86,342.6mg/kg,而重金属元素Ni,Cd,Cr,Pb未检出。用此法节省时间和试剂,环境污染少,操作简便,精密度和准确度较高。