Chromium content in selected convenience and fast foods in Poland

The chromium content in selected convenience and fast foods was determined. Samples were wet digested with HNO₃ (69%) in a microwave digestion system. Chromium was determined by graphite furnace atomic absorption spectroscopy (GF-AAS). The chromium content in convenience food ranged on average from 2.22 to 18.2 μg/100 g, in fast food from 3.76 to 28.6 μg/100 g, and in instant food from 0.34 to 4.75 μg/100 g.     

Monitoring multi-class pesticide residues in fresh grape by hollow fibre sorptive extraction combined with gas chromatography–mass spectrometry

A fast and sensitive multi-residue analysis method is reported for simultaneous determination of 25 pesticides of chemical classes which are spiked into fresh grape. The sample pretreatment method involves extraction and clean-up in one step with SiO₂ hollow fibre from 1.0 mL fresh grape slurry to minimise the matrix effects, and determination by gas chromatography–mass spectrometry with selective ion monitoring mode. The validation of the optimised method in terms of linearity, precision, recovery and repeatability showed that the proposed procedure is sensitive (the limits of detection were in the range of 0.0009–0.0084 μg mL⁻¹ for 25 pesticides), precise and repeatable (average recoveries were between 61% and 108% with relative standard deviations from 4.0% to 12.4 %). The proposed method was also applied to the analysis of these groups of pesticides in fresh grape sample purchased from the local markets of Lanzhou (China), while no residues of the selected pesticides were detected in the sample.     

Preconcentration and Trace Determination of Chromium Using Modified Ionic Liquid Cold-Induced Aggregation Dispersive Liquid–Liquid Microextraction: Application to Different Water and Food Samples

An efficient microextraction procedure based on modified ionic liquid cold-induced aggregation dispersive liquid–liquid microextraction (M-IL-CIA-DLLME) was developed for trace determination of chromium in water and food samples by flame atomic absorption spectrometry (FAAS), and it was used for speciation of Cr(III) and Cr(VI) in water samples by using Na₂SO₃ as the reducing agent. A mixture of water-immiscible 1-hexyl-3-methylimidazolium hexafluorophosphate ([Hmim][PF₆]) ionic liquid (IL) (microextraction solvent) and ethanol (disperser solvent) were directly injected into a heated aqueous solution containing bis(2-methoxy benzaldehyde) ethylene diimine as a Schiff’s base ligand (chelating agent), hexafluorophosphate (NaPF₆; as a common ion) and Cr(III). Afterwards, the solution was placed in an ice-water bath and a cloudy solution was formed due to a considerable decrease of IL solubility. After centrifuging, the sedimented phase containing enriched analyte was determined by FAAS. Under the optimum conditions, the calibration graph was linear over the range of 2–50 μg?L^?1 with limit of detection of 0.7 μg?L^?1. The accuracy of the present methodology was tested by recovery experiments and by analyzing a certified reference material. Relative standard deviation (RSD %) was 2.7 % for Cr(III). The proposed method was successfully applied for trace determination of chromium in water and food samples.     

Simultaneous multi-channel hydride generation atomic fluorescence spectrometry determination of arsenic,bismuth, tellurium and selenium in tea leaves

A novel, rapid and sensitive method for the simultaneous multi-channel hydride generation atomic fluorescence spectrometry (HG-AFS) determination of total arsenic (As), total bismuth (Bi), total tellurium (Te) and total selenium (Se) in tea leaves was proposed. The operating parameters of self-made multi-channel HG-AFS were optimised, including negative high voltage of photo multiplier tube (PMT), the flow rates of carrier and shield gas, observation height and lamp currents. The conditions of hydride generation for As, Bi, Te and Se were studied in details. Under optimal conditions, the method detection limits (MDL) for As, Bi, Te and Se in tea leaves were 0.0152 μg g⁻¹, 0.0080 μg g⁻¹, 0.0022 μg g⁻¹ and 0.0068 μg g⁻¹, respectively. The proposed method was successfully applied to the simultaneous determination of As, Bi, Te and Se in various tea leaves and the spike recoveries were in the range of 90–103%. The accuracy of method was validated by analysing a tea certified reference material. The obtained values were consistent with the certified ones.     

Ultra trace quantification of chromium(VI) in food and water samples by highly sensitive catalytic adsorptive stripping voltammetry with rubeanic acid

A simple and highly selective and sensitive catalytic adsorptive stripping voltammetric procedure for determination of ultra trace levels of chromium(VI) on hanging mercury drop electrode is reported. The method is based on the adsorptive preconcentration of the Cr(III)–dithiooxamide (rubeanic acid) complex and the utilization of the catalytic reaction in the presence of nitrate. At optimized conditions the calibration graph is linear from 0.01 to 6 ng/ml and detection limit is 0.002 ng/ml for accumulation time of 50 s. The interference of some common ions was studied and this method has been applied to the determination of chromium in food and waste water samples with satisfactory results.     

Determination of macro and trace element in multivitamins preparations by inductively coupled plasma optical emission spectrometry with slurry sample introduction

A slurry sampling technique has been utilised for elemental analysis of multivitamins preparations using inductively coupled plasma-emission spectrometry (ICP-OES). For results comparison, samples were mineralised. Slurry concentration 0.1–0.2% m/v in 6% v/v HNO₃, was used. The calibration by water standard solutions, slurry standards and standard additions were tested for determination above-mentioned elements in slurries. The method offers good precision for macro elements (RSD ranged from 5% to 10%). For in-home control sample, the measured concentrations are in satisfactory agreement with independent laboratories. For the analysed multivitamin preparations, the found element concentration is compared to amount declared by producer. The concentrations of Ca, Mg, P, K, Fe, Mn, Zn, Cu and Cr, Ni, V were determined in the range 1000–100,000 and 5–50 μg g⁻¹, respectively. The slurry ICP-OES analysis was found to be suitable for quality control monitoring of multivitamin preparations and could be useful as a routine procedure.     

A simple and highly sensitive spectrophotometric determination of Cr(VI) in food samples by using 3,4-dihydroxybenzaldehydeisonicotinoylhydrazone (3,4-DHBINH)

A simple, rapid, sensitive and inexpensive method has been developed for the determination of trace amounts of chromium(VI) using 3,4-dihydroxybenzaldehydeisonicotinoylhydrazone (3,4-DHBINH). The metal ion gives a yellow coloured complex with 3,4-DHBINH in acetate buffer of pH 5.5 with 1:1 (metal:ligand) composition. The complex shows a maximum absorption at 400 nm. Beer’s law is obeyed in the range 0.5–7.7 ppm of Cr(VI). The molar absorptivity, Sandell’s sensitivity and detection limit were found to be 1.35 × 10⁴ L mol⁻¹ cm⁻¹, 0.0075 μg cm⁻² and 0.0045 μg mL⁻¹, respectively. The correlation co-efficient and regression co-efficient of the Cr(VI)–3,4-DHBINH complex were 0.99 and 0.12, respectively. Major cations and anions did not show any interference. The developed method has been successfully applied for the analysis of Cr(VI) in food samples (leafy vegetables), comparing the results simultaneously with those obtained using an Atomic Absorption Spectrophotometer, whereby the validity of the method has been tested.     

Electrochemical behaviour of Sudan I at Fe3O4 nanoparticles modified glassy carbon electrode and its determination in food samples

In this work, a simple and sensitive electrochemical method was developed to determine Sudan I based on magnetic Fe₃O₄ nanoparticles modified glassy carbon electrode using cyclic voltammetry and differential pulse voltammetry. The sensor exhibited an obviously electrocatalytic activity towards the oxidation of Sudan I, which can be confirmed by the increased oxidation peak current and the decreased oxidation peak potential when compared with the bare GCE. The determination conditions, such as pH, modifier amount, accumulation time and accumulation potential, were optimised. And some kinetic parameters were calculated. Under the optimum experimental conditions, the oxidation current of Sudan I was proportional to its concentration from 0.01 to 1 μM and 1 to 20 μM. The detection limit was estimated to be 0.001 μM (S/N = 3). The developed method was successfully applied to determine Sudan I content in food samples with satisfactory results.     

A simple classical wet digestion technique for the determination of total mercury in fish tissue by cold-vapour atomic absorption spectrometry in a low technology environment

Four classical wet digestion procedures for the determination of mercury (Hg) by cold-vapour atomic absorption spectrometry in fish tissue were investigated with the aim of selecting and optimising the most convenient and inexpensive for use in a low technology environment. A mixture of H₂O, HNO₃, HClO₄ and H₂SO₄ or a mixture of HCl, HNO₃, HClO₄ and H₂SO₄ was used for the digestion in two different vessels namely thick walled long neck 50 ml volumetric flask and 50 ml 26 mm × 200 mm pyrex test tube. The effect of temperature and time on the digestion efficiency of the mixture of HCl, HNO₃, HClO₄ and H₂SO₄ using test tubes were investigated to obtain the optimum conditions. Mercury was partly lost at temperatures above 230 °C and this was pronounced when decomposition time was more than 30 min. Detection limit for the optimised procedure was 0.52 ng g⁻¹. The optimised procedure was employed to study the level of Hg in canned fish samples. Concentration of Hg in the samples tested ranged from 0.015 to 0.139 μg g⁻¹ wet weight.     

Determination of lead and cadmium in food samples by the coprecipitation method

In this study, the coprecipitation method developed using a combination of 2-mercaptobenzothiazole (MBT) as a chelating reagent and copper as coprecipitate carrier was used for the determination of trace lead and cadmium in various food samples by graphite furnace atomic absorption spectrometry (GFAAS). The method was applied for the determination of Pb(II) and Cd(II) in salami, sausage, chicken, anchovy, spinach, cabbage, onion, dill, parsley, lettuce, tea and rice samples. The matrix modifiers were added as 50 μg NH₄H₂PO₄ + 3 μg Mg(NO₃)₂ for both Pb(II) and Cd(II). The signals were measured as peak area. The concentrations of Pb(II) and Cd(II) in the food samples were found to be in the range of 6.63 ng g⁻¹ (anchovy) −3.30 μg g⁻¹ (spinach) and 2.67 ng g⁻¹ (salami) −0.51 μg g⁻¹ (lettuce), respectively.     

Determination of chromium(VI) in black,green and herbal teas

Speciation analysis of black, green and herbal teas was carried out by treating the samples with 0.1 M Na₂CO₃ to determine total Cr(VI) and acid digestion (of tea samples in a microwave) was applied to determine the total chromium concentrations by graphite furnace atomic absorption spectrometry (GF-AAS). The Cr(VI) content that could be consumed per unit cup of tea was determined by soaking the leaf or tea bag (or infusion) in 200 mL boiled water and the solution was filtered through a PDVF 0.45 μm hydrophilic filter prior analysis by GF-AAS.     

Effect of modifiers for As,Cu and Pb determinations in sugar-cane spirits by GF AAS

Palladium plus magnesium nitrates with and without Ir, Ru and W were evaluated for the simultaneous determination of As, Cu and Pb in cachaça by graphite furnace atomic absorption spectrometry. For 20 μL of sample, 5 μL Pd(NO₃)₂ and 3 μL Mg(NO₃)₂ dispensed together onto the Ir-coated platform of the THGA, analytical curves in the 0–30.0 μg L⁻¹ As, 0–1.50 mg L⁻¹ Cu and 0–60.0 μg L⁻¹ Pb were built up and typical linear correlation coefficients were always better than 0.999. The limit of detection was 1.30 μg L⁻¹ As, 140 μg L⁻¹ Cu and 0.90 μg L⁻¹ Pb. As, Cu and Pb contents in 10 cachaça samples agreed with those obtained by ICP-MS. Recoveries of spiked samples varied from 96% to 106% (As), 97% to 112% (Cu) and 92% to 108% (Pb). The relative standard deviation (n = 12) was typically 2.7%, 3.3% and 1.9%.     

Use of Cu(II) and Fe(III) N-benzoyl-N-phenylhydroxylamine coprecipitants for preconcentration of some trace metal ions in food samples

In this study, new coprecipitation methods were developed using a combination of N-benzoyl-N-phenylhydroxylamine (BPHA) as a chelating reagent and copper(II) and iron(III) as coprecipitate carriers. The determinations of Fe(III), Cr(III) and Cr(VI) with Cu(II)–BPHA coprecipitant and of Cu(II), Pb(II), Cr(III) and Cr(VI) with Fe(III)–BPHA coprecipitant were made by flame atomic absorption spectrometry. The surface morphology of coprecipitants was examined by scanning electron microscopy. The coprecipitation conditions for each method such as the effect of pH, the amounts of carrier element and BPHA, sample volume and matrix effects were examined. The optimum pH for each method was found to be 6. The detection limits of the methods changed in the range of 0.23–3.2 μg L⁻¹ with an enrichment factor of 100. The RSD % was ?4.2. The accuracy of the methods was confirmed by analysing the certified reference material. The developed methods were applied for the determination of analytes in food samples.     

Cloud point extraction for speciation of iron in beer samples by spectrophotometry

A new method based on the cloud point extraction (CPE) separation and spectrophotometric detection was proposed for the determination of iron species. In this method, Fe(II) reacts with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) in the presence of EDTA yielding a hydrophobic complex, which then is extracted into surfactant-rich phase. Total iron was determined after the reduction of Fe(III) to Fe(II) by using ascorbic acid as reducing agent. Variable parameters affecting the CPE efficiency were evaluated and optimised. The calibration graph was linear in the range of 5.0–112 μg/L (at 742 nm) for both species. Under the optimised conditions, the detection limits of 0.8 μg/L and 1.0 μg/L and the relative standard deviations of 2.0% and 2.6% (C_Fe(II) = C_Fe(III) = 10 μg/L, n = 5) for Fe(II) and Fe(III) were found, respectively. The proposed method has been applied to the speciation of iron in beer samples with satisfactory results.     

Synthesis and application of a new functionalized resin for use in an on-line,solid phase extraction system for the determination of trace elements in waters and reference cereal materials by flame atomic absorption spectrometry

The synthesis and characterization of the resin Amberlite XAD-4 functionalized with 2,6-pyridinedicarboxaldehyde and its application in an on-line system for the preconcentration of cadmium, cobalt, copper, lead and manganese prior to determination using flame atomic absorption spectrometry (FAAS) is proposed. Metal ions retained on the modified resin were eluted using 1.0 mol L⁻¹ HNO₃ solution and aspirated directly to the nebulizer–burner system of a FAAS instrument using a flow injection system. Detection limits (3σ) were determined to be 0.13 μg L⁻¹ for Cd, 0.29 μg L⁻¹ for Cu, 0.23 μg L⁻¹ for Mn, 0.58 μg L⁻¹ for Co and 2.19 μg L⁻¹ for Pb using a 10 mL of water sample loading volume. The limits of detection would be 100 times higher with units of μg kg⁻¹ for the solid samples in which their dilution ratios as (volume/weight) were 100. Enrichment factors ranged from 23.6 to 28.9 (for Co and Mn, respectively). The proposed method was successfully applied to determination of the analytes in natural water samples and certified reference materials.     

Development of polyclonal antibody-based indirect competitive enzyme-linked immunosorbent assay for sodium saccharin residue in food samples

A sensitive and specific polyclonal antibody (PcAb)-based indirect competitive enzyme-linked immunosorbent assay (icELISA) for sodium saccharin is described. 6-Amino saccharin was coupled to carrier protein for artificial antigen by diazotisation. New Zealand white rabbits were immunised to obtain anti-sodium saccharin PcAb and then icELISA was developed. The assay showed high sensitivity and specificity to sodium saccharin, with the 50% inhibition value (IC₅₀) of 0.243 μg mL⁻¹, workable range (IC₃₀–IC₇₀) of 0.050–12.8 μg mL⁻¹ and limit of detection (LOD, IC₂₀) of 0.021 μg mL⁻¹. The average recoveries of sodium saccharin in spiked food samples were estimated ranging from 70.7% to 98.8%. A statistically significant correlation of results was obtained between this new ELISA and previously established HPLC approaches with the food-relevant sodium saccharin concentration range 0–320 μg mL⁻¹ (R² = 0.9887–0.9975). These results indicated that the established ELISA was a potential and useful analytical tool for rapid determination of sodium saccharin residue in food samples.     

Tungsten permanent chemical modifier with co-injection of Pd(NO3)2 + Mg(NO3)2 for direct determination of Pb in vinegar by graphite furnace atomic absorption spectrometry

A tungsten carbide coating on the integrated platform of a transversely heated graphite atomizer (THGA^®) used together with Pd(NO₃)₂ + Mg(NO₃)₂ as modifier is proposed for the direct determination of lead in vinegar by graphite furnace atomic absorption spectrometry. The optimized heating program (temperature, ramp time, hold time) of atomizer involved drying stage (110 °C, 5 s, 30 s; 130 °C, 5 s, 30 s), pyrolysis stage (1000 °C, 15 s, 30 s), atomization stage (1800 °C, 0 s, 5 s) and clean-out stage (2450 °C, 1 s, 3 s). For 10 μL of vinegar delivered into the atomizer and calibration using working standard solutions (2.5–20.0 μg L⁻¹ Pb) in 0.2% (v/v) HNO₃, analytical curve with good linear correlation (r = 0.9992) was established. The characteristic mass was 40 pg Pb and the lifetime of the tube was around 730 firings. The limit of detection (LOD) was 0.4 μg L⁻¹ and the relative standard deviations (n = 12) were typically <8% for a sample containing 25 μg L⁻¹ Pb. Accuracy of the proposed method was checked after direct analysis of 23 vinegar samples. A paired t-test showed that results were in agreement at 95% confidence level with those obtained for acid-digested vinegar samples. The Pb levels varied from 2.8 to 32.4 μg L⁻¹. Accuracy was also checked by means of addition/recovery tests and recovered values varied from 90% to 110%. Additionally, two certified reference materials were analyzed and results were in agreement with certified values at a 95% confidence level.     

Determination of Allura red in food samples after cloud point extraction using mixed micelles

A cloud point extraction process using mixed micelles of CTAB, Triton X-114 and Triton X-100 for preconcentration and spectrophotometric determination of trace amounts of Allura red in food samples was developed. The effect of different parameters such as concentration of surfactants, electrolyte concentration, temperature and pH on the cloud point extraction of Allura red was studied in detail and a set of optimum conditions were established. A linear calibration curve in the range of 20–1400 μg/L of Allura red was obtained. Detection limit based on 3S_b was 7.8 μg/L and the relative standard deviation for 75 μg/L of Allura red was 3.87 (n = 10). The method was applied to the determination of Allura red in food samples such as candy, soft drink and jellies.     

Evaluation of the influence of arsenical livestock drinking waters on total arsenic levels in cow’s raw milk from Argentinean dairy farms

The concentrations of total arsenic in cow’s raw milk and in the livestock drinking water were determined and compared, in order to establish the influence of natural arsenic levels in groundwaters on the final presence of arsenic in milk production of the most important dairy region in Argentina. A dry ashing procedure was used for the mineralisation of the milk samples. The total arsenic concentrations were determined by flow injection hydride generation atomic absorption spectrometry (FI-HGAAS). The mineralised milk samples and well water samples were pre-reduced with concentrated HCl and KI–C₆H₈O₆ solutions. A volume of 500 μl of each solution of pre-treated sample was transported by a HCl 1.2 mol l⁻¹ carrier solution at a flow rate of 11 ml min⁻¹ and merged with a reducing NaBH₄ 0.2% (m/v) solution which flowed at 5.5 ml min⁻¹. The hydride generated in a reaction coil was transported to the detector with a N₂ flow of 100 ml min⁻¹. The recovery values of added concentrations at levels of 2.5 μg l⁻¹ and 5.0 μg l⁻¹ of arsenic in milk were 103 ± 8% and 102 ± 6% for n = 3, respectively. The accuracy of the method for the determination of total arsenic in water was checked by analysis of a certified sample NIST 1643d. Detection limits were 0.7 μg l⁻¹ and 0.6 μg l⁻¹ for milk and well water, respectively. The results showed a low biological transference level of arsenic to the cow milk from the drinking water ingestion.     

Fumonisin level in corn-based food and feed from Linxian County,a high-risk area for esophageal cancer in china

The level of mycotoxin fumonisins in corn-based food and feed collected from Linxian County, a high-risk area for esophageal cancer in China, has been analyzed using high-performance liquid chromatographic coupled with evaporative laser scattering detector (HPLC-ELSD). A total of 104 corn kernel samples were obtained from local households, granaries, wholesale markets (central markets), and retail markets (stores and supermarkets). Fumonisin B₁ (FB₁) was detected in the samples from households, granaries, central markets, and stores, with a positive rate of 61.5%, 50%, 33.3%, and 17%, respectively. No fumonisin was detected in samples from the supermarket. The highest FB₁ levels (0.30–3.20 μg/g; mean, 1.42 μg/g) were found in samples from the granary, followed by household (0.25–1.80 μg/g; mean, 0.73 μg/g), central market (0.25–1.10 μg/g; mean, 0.51 μg/g), and store (0.22–0.34 μg/g; mean, 0.28 μg/g). Among the 80 corn kernel samples collected from local households, 18 of 24 (75.0%) moldy samples contained high levels of FB₁ (0.28–3.30 μg/g; mean, 1.58 μg/g), and 20 of 56 (35.7%) apparently healthy samples contained low levels of FB₁ (0.21–0.82 μg/g; mean, 0.46 μg/g). As the central market plays an important role in trade of corn-based food and feed in China, a total of 115 corn-based food and feed samples were collected from the local central market. The highest FB₁ levels (0.30–3.13 μg/g; mean, 1.50 μg/g) were found in feed, followed by unprocessed food (0.31–0.63 μg/g; mean, 0.47 μg/g) and processed food (0.21–0.28 μg/g; mean, 0.25 μg/g). The positive incidence of FB₁ in feed, unprocessed, and processed food were 53.6%, 33.3% and 17.9%, respectively. In conclusion, the results showed that corn-based food and feed from Linxian County contained low level of FB₁ (<2 μg/g) in general, but efforts should be made to control the fumonisin contamination in corn kernels stored in granaries and households.