Trace element levels in raw milk from northern and southern regions of Croatia

A total of 157 raw milk samples were collected from tankers arriving at processing facilities from rural areas in northern and southern regions of Croatia during 2009 and 2010. Concentrations of As, Cd, Cu, Hg and Pb in the samples were analysed by graphite furnace-atomic absorption spectroscopy. Mean Pb concentrations in northern and southern regions were 58.7 and 36.2 μg l⁻¹, respectively, and both exceeded the maximum recommended level. Arsenic concentrations ranged from 1 to 283 μg l⁻¹ in the southern and to 1019 μg l⁻¹ in the northern regions. Mean Cd and Hg levels were: 1.76 and 1.59 in the northern and 3.4 and 7.1 μg l⁻¹ in the southern region. Significantly higher Cd and Hg levels were observed in the southern than in the northern region (p < 0.001, both). Similar mean Cu levels were found in both regions: 931.9 in the north and 848.4 μg l⁻¹ in the south. The results indicate that particular attention should be paid to Pb residues. In future studies, a greater number of milk samples and grass samples from pastures from different regions of Croatia should be controlled to confirm the absence of possible toxicological risks.     

Evaluation of trace element contents in canned foods marketed from Turkey

Trace element contents of 10 canned foods (mushroom, corn, pea, mixed vegetable, tomato, red mullet, stuffed grape leaves, pickle, bean, delicatessen) from Turkish markets were determined by flame and graphite furnace atomic absorption spectrometry after microwave digestion. The accuracy of the method was determined by use of a standard reference material (NIST SRM 1573a Tomato Leaves). The contents of investigated trace elements in canned foods were found to be in the range of 2.85–7.77 μg/g for copper, 8.46–21.9 μg/g for zinc, 6.46–18.6 μg/g for manganese, 27.5–79.6 μg/g for iron, 0.05–0.35 μg/g for selenium, 0.93–3.17 μg/g for aluminium, 0.19–0.52 μg/g for chromium, 0.18–0.75 μg/g for nickel, and 0.20–1.10 μg/g for cobalt. The results found were compared with those reported by scientists from various countries.     

Determination of trace element contents of baby foods from Turkey

The levels of trace elements in different types of baby foods consumed in Turkey were determined by flame and graphite furnace atomic absorption spectrometry. Dry, wet and microwave digestion procedures were compared and the microwave digestion method was found to be the best. The accuracy of the method was ensured by using a standard reference material (NIST-SRM 8418 Wheat Gluten). The levels of elements in analyzed samples were found to be under legal limits. The range of the investigated elements were 0.52–4.38 μg/g, 0.22–7.20 μg/g, 1.02–67.5 μg/g, 0.92–37.2 μg/g, 0.12–0.32 μg/g, 2.02–68.8 μg/kg, 10.7–66.8 μg/kg, 0.05–10.3 μg/g, 2.67–25.4 μg/kg for Cu, Mn, Fe, Zn, Se, Cr, Al, Ni and Co, respectively.     

Mineral and trace metal levels in some cheese collected from Turkey

Concentrations of elements (Fe, Mn, Zn, Cu, Pb, Cr, Ni, Na, K, Ca and Mg) in cheese samples were analyzed using flame and graphite furnace atomic absorption spectrometry after microwave digestion. The order of levels of the elements in the samples was determined to be Na > Ca > K > Mg > Zn > Fe > Pb > Mn > Cr > Ni. The concentration ranges in the samples were found to be 4.1–12.5, 0.28–1.1, 8.8–13.2, 0.10–0.27, 0.14,–1.2, 0.02–0.62, 0.18–0.34, 3957–6558, 305–362, 3473–4556 and 28.9–127 μg/g for iron, manganese, zinc, copper, lead, chromium, nickel, sodium, potassium, calcium and magnesium, respectively. High trace metal and mineral accumulation levels in the samples were found in Van otlu cheese for Fe, Ordu çerkez cheese for Na, Kayseri çömlek cheese for Mn, Pb, Çeçil cheese for Zn, Kars ka?ar cheese for Cu, Cr, Tokat cheese for Ni, Ca and Erzincan tulum cheese for K, Mg, respectively.     

Determination of toxic and essential elements in sunflower honey from Thrace Region,Turkey

The aim of this study was to determine the levels of copper (Cu), manganese (Mn), zinc (Zn), iron (Fe), cadmium (Cd), lead (Pb), chromium (Cr), nickel (Ni) and selenium (Se) in sunflower honeys obtained from Thrace Region of Turkey. Trace and toxic element determination was performed by atomic absorption spectrometry after microwave digestion. The accuracy of the method was checked by the standard reference material, NIST‐SRM 1515 Apple leaves. The maximum contents of trace and toxic elements in honey samples from Kesan (polluted area) were found as 0.46, 0.82, 1.98, 14.0, 9.86 μg kg^?1, 0.48 mg kg^?1, 137, 115 and 290 μg kg^?1 for Cu, Mn, Zn, Fe, Cd, Pb, Cr, Ni and Se, respectively.     

Determination of trace metals in canned fish marketed in Turkey

The levels of trace metals of canned fish samples collected from markets in Turkey were determined by flame and graphite furnace atomic absorption spectrometry after microwave digestion. The accuracy of the method was corrected by standard reference material (NRCC-DORM-2 Dogfish Muscle). The contents of investigated trace metals in canned fish samples were found to be in the range 1.10–2.50 μg/g for copper, 7.57–34.4 μg/g for zinc, 0.90–2.50 μg/g for manganese, 10.2–30.3 μg/g for iron, 0.96–3.64 μg/g for selenium, 0.45–1.50 μg/g for aluminium, 0.97–1.70 μg/g for chromium, 0.42–0.85 μg/g for nickel, 0.09–0.40 μg/g for lead and 0.06–0.25 μg/g for cadmium. The results were compared with the literature values.     

Trace metal content in nine species of fish from the Black and Aegean Seas,Turkey

Trace metal content of nine fish species harvested from the Black and Aegean Seas were determined by microwave digestion and atomic absorption spectroscopy (MD–AAS). Verification of the MD–AAS method was demonstrated by analysis of standard reference material (NRCC-DORM-2 dogfish muscle). Trace metal content in fish samples were 0.73–1.83 μg/g for copper, 0.45–0.90 μg/g for cadmium, 0.33–0.93 μg/g for lead, 35.4–106 μg/g for zinc, 1.28–7.40 μg/g for manganese, 68.6–163 μg/g for iron, 0.95–1.98 μg/g for chromium, and 1.92–5.68 μg/g for nickel. The levels of lead and cadmium in fish samples were higher than the recommended legal limits for human consumption.     

Determination of trace metal levels in sediment and five fish species from lakes in Tokat,Turkey

In this study, concentrations of trace metals in five fish species (Cyprinus carpio, Capoeta tinca, Leiciscus cephalus, Carassius gibelio and Silurus glanis) and sediments collected from some lakes in Tokat were determined by atomic absorption spectrometry. The fish species and sediment samples were collected from six lakes (Bedirkale, Boztepe, Belp?nar?, Avara, Ataköy and Ak?n) in Tokat, Turkey in spring and summer during 2003–2004. The samples were digested with a microwave digestion system. The maximum Fe, Mn, Zn, Cu, Pb, Cr and Ni concentrations of sediment samples were 2138, 232, 38.9, 8.2, 7.0, 10.7 and 55.4 μg/g, respectively. The maximum Fe, Zn, Cu, Pb, Cr, Mn and Ni concentrations of the fish samples were 167, 48.6, 3.6, 2.8, 1.6, 64.3 and 5.6 μg/g, respectively.     

Investigation by ICP-MS of trace element levels in vegetable edible oils produced in Spain

The content of trace elements (Ag, As, Ba, Be, Cd, Co, Cr, Cu, Fe, Hg, Mn, Mo, Ni, Pb, Sb, Ti, Tl and V) in edible oils (virgin olive, olive, pomace-olive, sunflower, soybean and corn) from Spain was determined, using inductively-coupled plasma-mass spectrometry (ICP-MS) after microwave digestion, employing only nitric acid in this step. The method has been validated by using both an oil reference material and recovery experiments over different oil samples, obtaining satisfactory results in all cases. Inter-day repeatabilities lower than 10% were observed for all of the analysed elements in the different kinds of oil samples. Studying the content of trace elements, in order to detect tendencies in the samples of the same type of oil, principal components analysis was used. Promising groupings were observed using a model with two principal components and retaining 75.3% of the variance.     

Matrix importance in animal material pre-treatment for metal determination

A relatively cheap and accessible way to analyze difficult samples without loss of analyte was optimized for determination of Cd, Cr, Cu, Hg, Ni, Pb, V and Zn in animal material. Reference materials with suitable matrix were used: Dorm-2 (Dogfish Muscle), Tort-2 (Lobster Hepatopancreas), and SRM 2976 (Mussel Tissue). The analytical procedure included digestion of the sample in Parr reactor bombs combined with a commercial microwave oven and metals analysis by atomic absorption spectrometry. A weak digestion procedure was optimized to prevent metal losses: a two-step digestion with an aqueous solution of HNO₃, each step carried at a microwave power of 340 W during 4 min. With the optimized procedure, metals concentrations in all reference materials matched certified ones (for a 95% level of confidence) with the exception of Cd in Tort-2 and Hg in SRM 2976. The present work reinforces the need to use matrix-matched reference materials and that any digestion protocol needs to be modified to maximize recoveries.     

Evaluation of trace and toxic element concentrations in Paris polyphylla from China with empirical and chemometric approaches

Trace and toxic elements in Paris polyphylla samples were determined by flame and graphite furnace atomic absorption spectrometry following microwave-assisted acid digestion, based on a mixture of nitric acid and hydrogen peroxide. The whole procedure, including sample preparation, digestion and measurements, was successfully validated against CRM GBW07603 (bush twigs and leaves). In order to get a better insight into the elemental patterns, common chemometric approaches to data evaluation, such as principal component analysis (PCA) and hierarchical cluster analysis (HCA), were used as classification techniques. Five significant groups classified by PCA were attributed partly to significant influential sources. HCA revealed five groups of P. polyphylla samples based on their trace and toxic element concentrations.     

Mineral and trace element content of various vegetarian foodstuffs available in Belgium

 Atomic absorption spectrometry was used to determine mineral (Na, K, Ca and Mg) and trace element content (Zn, Fe, Cu and Si) of various vegetarian foodstuffs in Belgium. Thirty-five commercially available products were analysed after a wet-acid destruction in a closed-vessel destruction bomb. Various important sources of the minerals and trace elements were identified. Since data for vegetarian foods in Belgium are non-existent, the concentration values are compared with the scarce literature data and particularly with levels found in the same products available in The Netherlands. Received: 2 June 1998 / Revised version: 5 October 1998     

微波消解-原子吸收法测定酥油粉中微量元素

本研究以消化温度、消化时间和消化压力为三个考察因素设计正交试验,对实验室自制微胶囊酥油粉进行微波消化。用火焰原子吸收光谱法对样品中的Ca、Mg、Fe、Cu、Zn五种元素进行测定。结果表明,最佳消化条件为:消化温度200℃,消化时间5min,消化压力15atm。在最佳实验条件下,对酥油粉各元素的含量做了回收实验,回收率范围在94.1%～105.1%,相对标准偏差0.41%～3.78%(n=6)。     

Variation in accumulation of heavy metals in different verities of sunflower seed oil with the aid of multivariate technique

In this work, three heavy metals (HMs) cadmium, lead, and zinc were determined in 16 newly breaded varieties of sunflower seed oil, using atomic absorption spectrometry, prior to use of microwave-assisted acid digestion method (MWD). The accuracy of the proposed method was studied by standard addition method and values obtained by conventional wet acid digestion methods (CAM) on same samples. The detection limit obtained from the standard addition curve was 0.327, 3.38, 10.0 ng/ml for Cd, Pb, and Zn, respectively, with high percentage recoveries. Multivariate statistical techniques (cluster and principal component analysis) were applied to modeling classes of different varieties of sunflower seed oils grown in same agricultural plot, on the basis of the analytical data of HMs. The results obtained providing sufficient information on tolerable limit of all three HMs by different varieties of sunflower oil to grow safely.     

微波消解-电感耦合等离子体质谱法 测定畜禽粪便中8种金属元素

目的建立微波消解-电感耦合等离子体质谱法(microwave digestion-inductively coupled plasma mass spectrometry, ICP-MS)测定畜禽粪便中8种金属元素的含量。方法干燥后的畜禽粪便样品经高速球磨仪球磨匀,采用微波消解仪对样品进行消解,消解后的样品用ICP-MS混合模式测定畜禽粪便中的砷、汞、铅、镉、铬、锌、铜和镍等8种金属元素,内标法定量。结果 8种元素检出限分别在0.017～0.64μg/L之间,线性关系良好,相关线性系数r0.999;不同元素的添加回收率为92.0%～101.9%,相对标准偏差为0.9%～5.0%。结论该方法样品前处理简单高效、分析用时短、准确度和精密度高,适用于批量畜禽粪便中多元素的测定。     

不同基质食品中总砷含量检测的2种前处理方法比较

目的比较湿法消解和微波消解2种前处理方法的处理效果,选择适合不同基质食品中总砷测定的前处理方法。方法分别采用湿法消解和微波消解的方法对样品进行前处理,利用氢化物-原子荧光光谱法测定紫菜粉、扇贝、大米粉和鸡肉中总砷的含量。结果砷的质量浓度在2~20μg/L内与其对应的荧光强度呈线性关系,方法检出限为0.0068 mg/kg,加标回收率为91.5%~99.6%,所有测定值的相对标准偏差(relative standard deviation,RSD)(n=4)均小于5%。紫菜和扇贝湿法消解测定的总砷结果在参考值范围内,微波消解测定的总砷结果明显低于参考值;大米和鸡肉用微波和湿法消解测定的总砷结果均在参考值范围内。结论对于海产品等砷存在形态复杂的食品中总砷的测定,适合采用湿法消解进行前处理,而对于砷存在形态相对简单的食品,微波和湿法消解均适用。     

微波消解-氢化物发生双道原子荧光光谱法同时测定糖蜜中的砷和汞

建立了微波消解-氢化物发生双道原子荧光光谱法同时测定糖蜜样品中砷和汞的分析方法。实验探索了酸的种类比例、固液比、微波强度、消解时间等各种微波消解条件,并对工作条件进行了优化。仪表检出限为砷0.0704μg/L,汞0.0089μg/L;精密度为砷1.13%,汞0.49%;样品加标回收率为砷96.1%～107.6%,汞102.3%～105.1%。应用该方法对广西某制糖集团下属公司的糖蜜中砷和汞的含量进行了分析,结果令人满意。     

A fast and simple methodology for determination of yttrium as an inert marker in digestibility studies

The need to develop a fast, simple and low cost methodology for the determination of yttrium in fish diets and faeces using a microwave digestion system and atomic absorption spectrometry with flame atomization analysis was the main aim of this study. The final methodology consisted in the digestion of approximately 300 mg of dry fish diet or 100 mg of dry fish faeces in teflon vessels using Parr reactor bombs, at high pressure, in a domestic microwave system with nitric acid solution. After digestion, 330 μl of a 120 mg potassium nitrate/ml solution was added to each solution. Yttrium was determined using a calibration with aqueous standards. Analytical difficulties and problems encountered during the optimizations were overcome and the application of the final methodology to the fish diets and faeces samples was carried out with suitable results.     

红枣微量元素含量测定分析

利用微波消解-原子吸收分光光度法,测定分析红枣中微量元素含量,发挥不同品种红枣的药用和食用价值。红枣中6种微量元素含量分别是:铁21.01mg/kg～31.09mg/kg,钙607.40mg/kg～787.80mg/kg,铜1.97mg/kg～3.58mg/kg,锌6.46 mg/kg～14.91mg/kg,锰2.64 mg/kg～3.67 mg/kg,镁358.60 mg/kg～431.40 mg/kg。结果表明:红枣中微量元素的含量丰富,尤其是钙、镁、铁的含量较高。