Total content of As,Sb, Se,Te and Bi in Spanish vegetables,cereals and pulses and estimation of the contribution of these foods to the Mediterranean daily intake of trace elements

As, Sb, Se, Te and Bi were quantified in vegetables, pulses and cereals, in order to increase the available information on the presence of these elements in the Mediterranean daily intake. Samples were dry ashed and the ashes dissolved with diluted HCl. Hydride generation atomic fluorescence spectrometry was used for quantification. Limits of detection (LOD) ranged from 0.2 to 1.7 ng g⁻¹ and the accuracy was assessed by the analysis of three certified reference materials, Rice Flour (NIST 1568a), Tomato Leaves (NIST 1573) and Cabbage (IAEA 359). Good concordance between results found and certified values were always observed. As, Sb, Se, Te and Bi levels varied in samples analysed from values under the LOD till 1001, 47, 270, 104 and 48 ng g⁻¹, respectively.     

Non-chromatographic speciation of inorganic arsenic in mushrooms by hydride generation atomic fluorescence spectrometry

A non-chromatographic speciation method has been developed for the determination of inorganic arsenic in cultivated and wild mushroom samples from different origins. The ultrasound-assisted extraction of the toxic arsenic species As (III) and As (V) was performed for 10 min with 1 mol l⁻¹ H₃PO₄ and 0.1% (m/v) Triton X-100. After phase separation the residue was washed with 0.1% (w/v) EDTA and centrifuged. As (III) and As (V) were determined by hydride generation atomic fluorescence spectrometry. Speciation was made using proportional equations corresponding to two different measurement conditions, (i) directly feeding sample extracts diluted with HCl and (ii) after reduction with KI and ascorbic acid for 30 min. The limits of detection of the method were 6.3 and 5.0 ng g⁻¹ for As (III) and As (V), respectively. Recovery percentages varied between 91% and 108% for As (III) and from 90% to 109% for As (V) indicating that As species interconversion was avoided. As (III) concentrations from 264 to 81 μg g⁻¹ and As (V) concentrations from 246 to 59 μg g⁻¹ were found in Spanish cultivated mushrooms. For Chinese wild mushrooms As (III) varied between 624 and 117 μg g⁻¹ and As (V) from 380 to less than 5 μg g⁻¹. The accuracy of the method was checked by the determination of total As (from the sum of As (III) and As (V)) in a tomato leaves reference sample, with good agreement with the certified value.     

Determination of ultratrace levels of selenium in fruit and vegetable samples grown and consumed in Portugal

The selenium content in fruit and vegetable samples from two regions in Portugal were analysed using hydride generation atomic fluorescence spectrometry (HG-AFS) and radiochemical nuclear activation analysis (RNAA) – two analytical methods with very low limits of detection. The lower detection limits of HG-AFS, 3 μg kg⁻¹ and 8 μg kg⁻¹ (according to conditions used for digestion), and for RNAA, 10 μg kg⁻¹, meant that it was possible to determine selenium in samples previously analysed using the replicate sample instrumental nuclear activation analysis (RSINAA) with a higher detection limit associated.     

Selenium species in buckwheat cultivated with foliar addition of Se(VI) and various levels of UV-B radiation

Common (Fagopyrum esculentum Moench) and tartary (Fagopyrum tataricum Gaertn.) buckwheat was treated by spraying the leaves with a water solution containing 15 mg Se per litre in the form of sodium selenate in the flowering period. The selenium content in all parts of plant was found to be less than 200 ng g⁻¹ in non-treated and in the range 2700–4650 ng g⁻¹ in selenium treated buckwheat. Exposure to UV-B radiation lead to higher Se accumulation in flowers of both Se enriched cultivars. For speciation analysis enzymatic hydrolysis was carried out, separation and detection of selenium species was performed by high performance liquid chromatography–ultraviolet treatment–hydride generation atomic fluorescence spectrometry (HPLC–UV–HG-AFS). In flowers and leaves, on average 11% of the Se content was soluble and in the form of Se(VI), representing between 0.6% (flowers) and 3% (leaves) of the Se content. The remaining soluble non-amino acid organic Se was not detected by HPLC–UV–HG-AFS. In seeds 93% of the selenium content was found in the extracts and the main selenium species was SeMet with 93 ± 5% relative to the selenium content.     

Trace element levels in honeys from different regions of Turkey

A survey of 25 honey samples from different botanical origin, collected all over the Turkey was conducted to assess their trace element contents. The aim of this study was to determine the levels of cadmium (Cd), lead (Pb), iron (Fe), manganese (Mn), copper (Cu), nickel (Ni), chromium (Cr), zinc (Zn), aluminium (Al) and selenium (Se) in honey samples from different regions of Turkey. Trace element contents were determined by a flame and graphite furnace atomic absorption spectrometry technique after dry-ashing, microwave digestion and wet-digestion. The accuracy of the method was corrected by the standard reference material, NIST-SRM 1515 Apple leaves. The contents of trace elements in honey samples were in the range of 0.23–2.41 μg g⁻¹, 0.32–4.56 μg g⁻¹, 1.1–12.7 μg g⁻¹, 1.8–10.2 μg g⁻¹, 8.4–105.8 μg kg⁻¹, 2.6–29.9 μg kg⁻¹, 2.4–37.9 μg kg⁻¹, 0.9–17.9 μg kg⁻¹, 83–325 μg kg⁻¹ and 38–113 μg kg⁻¹ for Cu, Mn, Zn, Fe, Pb, Ni, Cr, Cd, Al and Se, respectively. Iron was the most abundant element while cadmium was the lowest element in the Turkish honeys surveyed. The results showed that trace element concentrations in the honeys from different regions were generally correlated with the degree of trace element contamination of the environment.     

Comparison of isoflavones composition in seed,embryo, cotyledon and seed coat of cooked-with-rice and vegetable soybean (Glycine max L.) varieties

In order to study the content and composition of isoflavones retained in soybean seed component, obtained each component part the embryo, cotyledon and seed coat tissues of nine different soybean varieties were analyzed for 12 isoflavones using high performance liquid chromatography with photo diode array detector (HPLC-PDA) and were compared to each other. A total average concentration of isoflavone was 2887 μg g⁻¹ in embryo, 575 μg g⁻¹ in whole seed, 325 μg g⁻¹ in cotyledon, and 33 μg g⁻¹ in seed coat. With respect to each tissue of soybean varieties, isoflavone content was highest in Geomjeongkong 2 embryo (5701 μg g⁻¹), Geomjeongolkong whole seed (1321 μg g⁻¹), Heugcheongkong cotyledon (951 μg g⁻¹), and Keunolkong seed coat (56 μg g⁻¹). Isoflavone was least present in Keunolkong embryo (341 μg g⁻¹), Hwaeomputkong whole seed (175 μg g⁻¹), Seonheukkong cotyledon (81 μg g⁻¹), and Seoklyangputkong seed coat (5 μg g⁻¹). Overall, embryo and seed coat of all nine varieties contained isoflavones at the highest and lowest level, respectively. Isoflavones accumulated in the order of malonylglycoside, glycoside, acetylglycoside, and aglycon, among which malonylglycoside was the most abundant form ranging from 66% to 79% of the total isoflavone content in all three tissues. The embryo of cooked-with-rice soybean with black seed coat appears to be the best source of isoflavone.     

Effect of foliar application of selenium on its uptake and speciation in carrot

Carrot (Daucus carota) shoots were enriched by selenium using foliar application. Solutions of sodium selenite or sodium selenate at 10 and 100 μg Se ml⁻¹, were sprayed on the carrot leaves and the selenium content and uptake rate of selenium were estimated by ICP–MS analysis. Anion and cation exchange HPLC were tailored to and applied for the separation of selenium species in proteolytic extracts of the biological tissues using detection by ICP–MS or ESI–MS/MS. Foliar application of solutions of selenite or selenate at 100 μg Se ml⁻¹ resulted in a selenium concentration of up to 2 μg Se g⁻¹ (dry mass) in the carrot root whereas the selenium concentration in the controls was below the limit of detection at 0.045 μg Se g⁻¹ (dry mass). Selenate-enriched carrot leaves accumulated as much as 80 μg Se g⁻¹ (dry mass), while the selenite-enriched leaves contained approximately 50 μg Se g⁻¹ (dry mass). The speciation analyses showed that inorganic selenium was present in both roots and leaves. The predominant metabolised organic forms of selenium in the roots were selenomethionine and γ-glutamyl-selenomethyl-selenocysteine, regardless of which of the inorganic species were used for foliar application. Only selenomethionine was detected in the carrot leaves. The identity of selenomethionine contained in carrot roots and leaves was successfully confirmed by HPLC–ESI–MS/MS.     

Selective determination of copper and iron in various food samples by the solid phase extraction

The solid phase extraction method developed using N-benzoyl-N-phenylhydroxylamine as a chelating reagent and Amberlite XAD-1180 as an adsorbent was used for the determination of Cu(II) and Fe(III) in various food samples by flame atomic absorption spectrometry. The samples were digested by using nitric acid and hydrogen peroxide. The Cu concentrations ranged from 1.01 to 5.81 μg g⁻¹ in cereals, from 0.40 to 9.67 μg g⁻¹ in vegetable and fruits and from 0.37 to 0.70 μg g⁻¹ in infusions while the Fe concentrations ranged from 7.48 to 34.3 μg g⁻¹ in cereals, from 5.74 to 260 μg g⁻¹ in vegetable and fruits, from 1.63 to 5.12 μg g⁻¹ in infusions and from 0.24 to 1.56 mg L⁻¹ in beverage samples. The Cu and Fe concentrations found were compared with the results obtained from the other food studies in the world.     

Residue levels of food-grade antioxidants in postharvest treated in-pod peanuts during five months of storage

In order to investigate residue levels of butylated hydroxyanisole (BHA), propyl paraben (PP) and butylated hydroxytoluene (BHT) during storage, eight-hundred kilograms of bulk peanuts were treated with the following antioxidant emulsions: BHA (1802 μg g⁻¹), BHA–PP (1802 μg g⁻¹ + 1802 μg g⁻¹) M1 and BHA–PP–BHT mixtures (1802 μg g⁻¹ + 901 μg g⁻¹ + 2204 μg g⁻¹) M2 and (1802 μg g⁻¹ + 1802 μg g⁻¹ + 2204 μg g⁻¹) M3. Residues were determined in peanut pod and seed tissues at 1-month intervals during the storage. While the reduction levels of BHA and PP in pods at the end of the storage period ranged from 66% to 76%, BHT levels were decreased extensively (86%). Twenty-four hours after peanuts were treated, antioxidant emulsions effectively seeped into the seeds and low levels of these chemicals were detected during the assay. Residues of PP in seeds were lower (62%) than the other antioxidants. Although the doses used were higher than those approved for food-grade antioxidants in stored peanuts, the residue levels in seeds (32.8–0.02 μg g⁻¹) did not exceed the maximum residue limits during the storage period.     

Determination of methylmercury in marine and freshwater fish in Ghana using a combined technique of dithizone extraction and gas–liquid chromatography with electron capture detection

Concentrations of methylmercury (MeHg) residues were determined in different marine and freshwater fishes from Ghana. Samples were treated with ethanolic potassium hydroxide in water bath at 100 °C for 1 h. After neutralising with HCl and washing with hexane, MeHg was extracted with dithizone in toluene, cleaned up and determined by gas chromatography with electron capture detection (GC–ECD). The method was sensitive with good precision, detection limit of 0.0005 μg g⁻¹ (0.5 μg kg⁻¹) and provided good separation for organomercury compounds. The validity of the method was established using dogfish muscle certified reference material, DORM-2. The method was applied to different fish species. Concentration of MeHg in the edible muscle tissue of the tested fish ranged from 0.009 to 0.107 μg g⁻¹ wet weight. The concentrations of MeHg in the fish samples obtained do not however, constitute any significant mercury exposure to the general population through consumption of the tested fish species.