Major and trace elements levels in multifloral and unifloral honeys in Croatia

Different honey types were collected in Croatia during 2010 and 2011: 7 multifloral orchard honeys, 7 multifloral meadow honeys, 19 black locust, 9 chestnut, 11 lime and 6 sage honeys. Elements were measured using graphite (As, Cu, Cd, Pb, Se) and flame atomic absorption spectrometer (Ca, Fe, K, Mg, Na, Zn) and by mercury analyser (Hg). Significant differences in Ca, Fe, K, Mg, Zn, As and Hg levels were observed between honey types. In chestnut honey were determined (K, Ca, Mg: mg kg⁻¹; Hg, Ad, Cd: μg kg⁻¹): the highest concentrations of K 2824.4, Ca 486.7, Mg 59.1 and Hg 2.52; the lowest of As 24.1 and Cd 2.52. Lime honey has been shown the highest content of Cu (20.6 mg kg⁻¹), Zn (6.78 mg kg⁻¹), Cd (2.14 μg kg⁻¹) and Pb (810.3 μg kg⁻¹). The lowest levels of following elements were determined in black locust honey (Fe, K, Mg: mg kg⁻¹; Hg: μg kg⁻¹): Fe 2.77, K 304.7, Mg 8.02 and Hg 0.82. Sage honey had the lowest Ca and Na content (173.9 and 31.8 mg kg⁻¹). Among the multifloral honeys, the following was determined (Fe, Na, Cu: mg kg⁻¹; As, Pb: μg kg⁻¹): orchard honey – highest of Fe 5.17 and As 276.1, lowest Pb 301; meadow honey – highest Na 36.1, lowest Cu 4.38. The average Ca, Cu and Pb levels found in multifloral honey types were much higher than those reported in other European countries. Calcium levels in lime, chestnut and black locust were higher than those from other countries.     

Assessing arsenic,cadmium, and lead contents in major crops in Brazil for food safety purposes

The food chain is one of the major sources of human exposure to non-essential trace elements (TEs) present in soils. Human exposure to contaminated food is a worldwide health concern and a food safety issue that threatens agricultural trade. To assess the quality of Brazilian food products with respect to non-essential TEs, we evaluated arsenic (As), cadmium (Cd), and lead (Pb) contents in five major crops grown in Brazil: rice, wheat, corn, soybeans, and potatoes. The samples were collected from field trials with a record of long-term use of phosphate fertilizers in the states of Mato Grosso and Minas Gerais, Brazil. The TE concentrations in soils were all bellow the maximum allowable concentrations for agricultural soils. The mean concentrations of As, Cd, and Pb (μg kg⁻¹ dry weight) were as follows: below the detection limit <15, 29, and <40 for rice; 19, 23, and 64 for wheat; 47, 40, and 95 for corn; 65, 23, and 106 for soybeans; and 59, 22, and <40 for potatoes, respectively. Significant differences were found in the As and Cd contents of the different wheat cultivars. The levels of As, Cd, and Pb found in the studied crops are well below the values reported in the literature and are in accordance with the Codex Alimentarius and the European Union and Brazilian guidelines, indicating that the concentrations of these elements in the crops do not pose a risk to human health.     

Comparison of the chemical composition of British and Continental European bottled waters by multivariate analysis

The elemental composition of 37 bottled waters from the UK and continental Europe has been determined. Ca, K, Mg, Na, Al, As, Ba, Cd, Cr, Co, Cu, Fe, Mn, Mo, Ni, Pb, Sb, Sr, U, V and Zn were determined by ICP-OES and ICP-MS, in addition to inorganic and total organic carbon. The composition of all the waters analysed fell within the guideline values recommended by the World Health Organization. Na, Ca, Sr and Ba showed the widest variation in concentrations, ranging over two orders of magnitude. Levels of Fe were below the limit of detection (30 μg L⁻¹) in all samples analysed. Waters produced in the UK generally showed lower levels of most major elements and trace metals, with the exception of Ba (up to 455 μg L⁻¹). Italian waters showed the highest concentrations of Sr (3000–8000 μg L⁻¹) and U (8–13 μg L⁻¹), whereas waters produced in Slovakia and the Czech Republic showed the highest levels of Pb (0.7–4 μg L⁻¹). The use of multivariate analysis reveals an association between high alkaline metal content and high concentrations of As and Cr. There also appears to be a correlation between high Ca and Sr content and high levels of U. Analysis of variance (ANOVA) indicates that the composition of bottled water can be distinguished primarily by the country of origin, over other factors including the geological environment of the source. This would suggest that composition reflects, and is biased towards, consumer preferences.     

Element differences and evaluation of the dietary intake from farmed oysters and mussels collected at different sites along the Croatian coast of the Adriatic Sea

Concentrations of the macroelements Ca, Mg, K and Na, microelements Cr, Cu, Fe, Mn and Zn and toxic metals As, Cd, Hg and Pb were determined in oysters and mussels collected at farming sites in the northern, central and south Adriatic Sea. Mean concentrations in oysters were (mg kg⁻¹): As 4.51, Ca 1551, Cd 1.44, Cu 53.6, Cr 0.23, Fe 45.9, Hg 0.047, K 2476, Mg 895, Mn 2.80, Na 7148, Pb 0.52, Zn 675. Mean values in mussels were (mg kg⁻¹): As 4.71, Ca 601, Cd 0.37, Cu 1.91, Cr 0.29, Fe 49.6, Hg 0.026, K 2246, Mg 1043, Mn 2.49, Na 7992, Pb 0.58, Zn 28.8. Significant differences in the concentrations of toxic metals and elements were found in oysters and mussels among farming sites. Obtained Cd, Hg and Pb concentration in oysters and mussels were lower than the limit levels set by the European Community. However, Cd concentration exceeded the limit level of 1 mg kg⁻¹ in oysters from all locations except Lim Bay. The estimated daily intakes (EDIs) indicate that oysters are a good source of Ca, Cu and Zn. The higher Cu and Zn concentrations than the toxicity reference values suggest a risk for consumers if larger quantities of oysters are consumed frequently.     

Genetic diversity of nutritionally important carotenoids in 94 pea and 121 chickpea accessions

Biofortification of staple crops via breeding is an attractive strategy for reducing human micronutrient deficiencies. The objective of this research was to examine the concentration of carotenoids in diverse pea and chickpea accessions grown in Saskatchewan (Canada) using high performance liquid chromatography. In pea accessions mean concentration of lutein was highest (11.2 μg g⁻¹) followed by β-carotene (0.5 μg g⁻¹), zeaxanthin (0.3 μg g⁻¹), and violaxanthin (0.3 μg g⁻¹). Green cotyledon pea accessions were richer in β-carotene and total carotenoids compared to yellow cotyledon accessions. In chickpea accessions mean concentration of lutein (8.2 μg g⁻¹) was highest followed by zeaxanthin (6.2 μg g⁻¹), β-carotene (0.5 μg g⁻¹), β-cryptoxanthin (0.1 μg g⁻¹), and violaxanthin (0.1 μg g⁻¹). Desi chickpea accessions had higher carotenoid concentration than kabuli accessions. This research identified pea and chickpea accessions that can be utilized in breeding for the improvement of carotenoid concentration through biofortification.     

Direct atomic absorption spectrometry determination of arsenic,cadmium, copper,manganese, lead and zinc in vegetable oil and fat samples with graphite filter furnace atomizer

The article presents the results of optimization of operation parameters, investigation of analytical characteristics and the abilities of a graphite filter-furnace (FF) atomizer for the direct electrothermal atomic absorption spectroscopy (ET AAS) determination of trace amounts of Mn, As, Pb, Cu, Cd and Zn in some vegetable oils and fats. The effect of pyrolysis and atomization temperatures of the graphite FF atomizer on atomic absorbance values of the listed elements at their evaporation from some organic solutions in the presence of a Pd-Mg chemical modifier (CM) was investigated. For the ET AAS determination of As, Pb, Cd and Zn with Pd-Mg CM, the temperature of the graphite FF atomizer for the pyrolysis step can be raised by 250–350 °C. This mode allows to eliminate the background absorption, to increase the sensitivity of the elements to be analyzed and to enhance the total content of vegetable oils or fats in organic solutions up to 0.5 g mL⁻¹. The obtained limits of quantification for Mn, As, Pb, Cu, Cd and Zn were 0.002, 0.004, 0.004, 0.002, 0.0008, 0.0004 mg kg⁻¹, respectively. The relative standard deviation (RSD) varied between ∼3 and 8% and the time of one element determination did not exceed ∼3–5 min. The reliability of the proposed method was checked using the reference method. A paired Student's t-test showed no significant difference between the results obtained by both methods on a 95% confidence level.     

A magnetic ion-imprinted polymer for lead(II) determination: A study on the adsorption of lead(II) by beverages

In this work a variety of beverage samples had been kept in a contaminated area to investigate their lead adsorption. To determine the adsorbed Pb(II), a novel magnetic lead ion-imprinted polymer, grafted onto Fe₃O₄ nanoparticles, was synthesized and used as a selective sorbent for the preconcentration of Pb(II) ions. The sorbent was characterized by different techniques. The synthesized sorbent was applied for highly accurate and selective determination of Pb(II) ions absorbed from polluted air in several beverages and results were compared. To validate the method, three certified reference materials were analyzed by the proposed method and the results showed that pre-concentrating by this sorbent and subsequent determination by flame atomic absorption spectroscopy is an accurate method for lead determination in beverage samples (recoveries higher than 95%). The limits of detection and the relative standard deviations were less than 1.7 μg kg⁻¹ and 4.1%, respectively. The sorption capacity of this new sorbent was 51.8 mg g⁻¹. Finally, this method was used for the determination of Pb(II) ions in polluted beverage samples, and the results revealed that under equal conditions, coffee exhibits more tendency to adsorb Pb(II) ions.     

Exposure assessment of arsenic speciation in different rice types depending on the cooking mode

Total (As_t), inorganic arsenic (As_i = As(III) + As(V)) and dimethylarsonic acid (DMA) were determined in 37 commercial rice samples collected in France. As_t was measured by inductively coupled plasma-mass spectrometry (ICP-MS) whereas anion-exchange chromatography – ICP-MS was used for As_i and DMA determination. As_t in raw rice varied from 0.041 to 0.535 mg kg⁻¹ whereas As_i varied from 0.025 mg kg⁻¹ (polished Basmati rice) up to 0.471 mg kg⁻¹ (organic rice duo). The daily intake and associated health risk for different population groups as a function of age and gender was also assessed. The intake varied between 0.002 and 0.184 μg kg⁻¹ body weight for As_t and 0.002 and 0.153 μg kg⁻¹ body weight for As_i, which do not pose a chronic toxicity risk. Organic wholegrain rice may entail a risk for children in the case of sole consumption at the expense of polished rice. The impact of rice cooking/boiling in terms of the overall toxicological risk related to As species was also investigated. Pre-rinsing and boiling the raw rice by using an excess of water is the most efficient mode to obtain a significant As_i removal and further reduction of the toxicological risk for children, particularly for white rice varieties.     

Bioactive compound composition of pomegranate fruits removed during thinning

Thinning consists of reducing fruit load at immature stage and thus allowing remaining fruits to develop to their maximum size and quality. The waste material produced during this farming practice was characterised in 9 pomegranate cultivars, by evaluating: weight, size, maturity index, pH, organic acids and sugars profiles, contents of minerals, punicalagin, and ellagic acid, total polyphenols and antioxidant activity. Citric and quinic were the main organic acids. Potassium was the predominant mineral, reaching up to 11 g kg⁻¹ dry weight (dw). Total polyphenol content ranged from 777 to 1660 g GAE kg⁻¹ dw, α-punicalagin from 101 to 195 and β-punicalagin from 80.1 to 111 g kg⁻¹ dw. The antioxidant activity was assessed by three methods and its values varied from 2923 to 4486 for ABTS, from 3153 to 4685 for FRAP, and from 2075 to 2934 mmol Trolox kg⁻¹ dw for DPPH. Pomegranate thinning fruits, especially sour-sweet cultivars, are rich in bioactive compounds, with a potential use in the food, chemical and pharmaceutical industries.     

Mineral composition and bioaccessibility in Sarcocornia ambigua using ICP-MS

This study evaluates the nutritional potential of Sarcocornia ambigua as new a source of minerals. The mineral concentrations of two different growing populations (natural occurrence and irrigated) of S. ambigua were evaluated using inductively coupled plasma mass spectrometry. In all samples, the mineral present in highest amounts was potassium (K) (19–24 μg g⁻¹), followed by magnesium (Mg) (8.6–14 μg g⁻¹) and then calcium (Ca) (2.6–4.0 μg g⁻¹). In addition, in vitro bioacessibility assay demonstrated that very high fraction (65–80%) of these K and Mg (80 and 65%) of total concentration of these elements is bioacessible from S. ambigua analyzed. The trace elements vanadium (V), chromium (Cr), cobalt (Co), copper (Cu) and lithium (Li) have more than above 50% of total concentration was found bioaccessible. In all cases, mass balance was verified by carrying out the total digestion of the remaining residue and the relationship between total concentration and bioaccessibility. The data related to the concentrations and the bioaccessible fractions of the minerals provide a starting point for more complex and in-depth evaluations from the nutritional point of view, including the establishment of a recommended daily dietary intake for this plant.     

Geographical discrimination of Italian honey by multi-element analysis with a chemometric approach

In this study the concentrations of K, Ca, Mg, Na, Al, Zn, Fe, Mn, Cu, Cr, Ni, Se, Pb, Cd, and As in 39 honey samples of different botanical (orange-blossom, lemon-blossom, chestnut, eucalyptus, acacia, sulla and wildflower honeys) and geographical (Sicily and Calabria, Italy) origin were determined by ICP-OES and ICP-MS. The most abundant minerals decreased in the following order: K (mean value: 1.57 mg g⁻¹) > Ca (0.2 mg g⁻¹) > Mg (0.121 mg g⁻¹) > Na (0.092 mg g⁻¹). Recommended Dietary Allowance (RDA) values and benchmark levels were employed to assess the honey quality and safety. The data excluded toxicological risks: for an adult of 60 kg, a daily intake of 2 g of honey covered maximum 0.40% of Tolerable Weekly Intake (TWI) for Al, 0.33% of Benchmark Dose of 1% Extra Risk (BMDL01) for Pb, and 0.07% of Tolerable Daily Intake (TDI) for Ni. Mineral content marks the differences in honey samples from different geographical origin despite the botanical factor weight and can be used as a tool to assess the traceability of honeys. The discrimination between Sicilian and Calabrian honeys was achieved by Principal Component Analysis (PCA), and also the results of Canonical Discriminant Analysis (CDA) indicate that the 100% of total samples are correctly classified. This research contributes to the studies to determine the geographical origin of honeys.     

Arsenic,cadmium, cobalt,copper, lead,mercury, molybdenum,selenium and zinc concentrations in liver,kidney and muscle in Australian sheep

Matched muscle, liver and kidney samples from 152 sheep in different states of Australia were analysed for trace elements. Mean levels found in muscle, livers and kidneys were 0.010, 0.010 and 0.011 mg kg⁻¹ (fresh weight) for arsenic; 0.0035, 0.280 and 0.853 mg kg⁻¹ for cadmium; 0.006, 0.060 and 0.044 mg kg⁻¹ for cobalt; 0.74, 66.0 and 2.72 mg kg⁻¹ for copper; 0.007, 0.040 and 0.057 mg kg⁻¹ for lead; 0.0025, 0.0034 and 0.0061 mg kg⁻¹ for mercury; 0.014, 1.05 and 0.44 mg kg⁻¹ for molybdenum; 0.09, 0.31 and 0.95 mg kg⁻¹ for selenium; and 40.4, 37.2 and 20.8 mg kg⁻¹ for zinc. The lead, mercury and arsenic concentrations in meat and organs may be regarded as low, but the concentrations of cadmium in kidney and livers are sometimes relatively high. Apart from cadmium, lead and selenium, tissue trace element concentrations were not related to the age of the investigated animals. Differences in essential and non-essential trace element accumulation in sheep reared in different regions (states and territories) of Australia were also evaluated. Cadmium, lead and selenium were the only elements that appeared to show significant regional differences. Overall the results show that concentrations of the elements considered are within current acceptable ranges.     

Single-run analysis of vitamin D photoproducts in oyster mushroom (Pleurotus ostreatus) after UV-B treatment

A single-run high performance liquid chromatography (HPLC) with diode array detector (DAD) based method was developed for the separation, identification and comprehensive quantification of degradation products of ergosterol formed in oyster mushroom (Pleurotus ostreatus) after UV-B exposure. After 60 min, 10 substances involved in the photoprocess were separated, identified by their characteristic DAD spectrum and distinguished by their molecular weight, in cases where spectra were identical: vitamin D₂, previtamin D₂, tachysterol₂, lumisterol₂ and ergosterol, and, in minor quantity, their structural analogues of the 22,23-dihydroergocalciferol (vitamin D₄) series. Sample preparation protocol affected the total yields and the ratios of previtamin and vitamin D₂/D₄. Hot alkaline hydrolysis resulted in the best digestion of the mushroom matrix and accordingly gave the highest vitamin D yield (D₂: 141.32 μg g⁻¹ dry matter, DM; D₄: 22.72 μg g⁻¹ DM). Limit of detection for vitamin D_2/4 was 0.02 μg g⁻¹ dry matter (DM) and was estimated for previtamin D_2/4 (0.06 μg g⁻¹ DM), tachysterol_2/4 (0.02 μg g⁻¹ DM) and lumisterol_2/4 (0.06 μg g⁻¹ DM). Recovery of spiked vitamin D₂ was 97 ± 0.7%. The study provides an analytical tool to assess the process of vitamin D generation after UV-B treatment for the production of oyster mushrooms with a balanced nutritional profile of vitamin D compounds.     

Heat-assisted slurry sampling GFAAS method for determination of lead in food standard reference materials

A valid method based on heat-assisted slurry sampling graphic furnace atomic absorption spectrometry (HASS-GFAAS) was developed for the accurate determination of trace Pb in food standard reference materials (SRMs). The HASS technique significantly improved Pb recovery and precision compared to conventional slurry sampling techniques. The optimized HASS procedure was performed as follows: first, the sample (particle size ≤ 150 μm) was diluted with 0.05% (v/v) Triton X-100 containing 2% HNO₃ and 1% H₂O₂ followed by heating for 20 min at 120 °C on a heating block. Next, the obtained slurry was sonicated in an autosampler cup, and finally, the slurry was introduced into a graphite tube and analyzed by the GFAAS with a Pb electrodeless discharge lamp (EDL). Calibration with aqueous standard solutions was used for Pb determination in food samples. The characteristic mass and limit of detection for Pb based on the integrated absorbance for a 2% (m/v) sample were 12 ± 0.6 pg and 0.003 mg kg⁻¹, respectively. The accuracy (95.1–102% recovery) and good precision (0.1–3.6%) of this procedure are illustrated by the results obtained for the 12 food reference materials. The proposed method is suitable for determination of trace Pb in solid food samples.     

Fluoroquinolone antibiotic determination in bovine milk using capillary liquid chromatography with diode array and mass spectrometry detection

A fast and sensitive method has been developed for the determination of five fluoroquinolones and a quinolone in commercial bovine milk by capillary-LC–DAD–MS after simple extraction method based on milk deproteinization with 15% trichloroacetic acid. Separation was carried out in a Zorbax SB-C18 column (150 mm × 0.5 mm, 5 μm) using a mixture of acetonitrile–5 mM ammonium formate (pH 3.7) as mobile phase in gradient elution mode. The sample was prepared in a 5 mM aqueous ammonium formate buffer for focusing purposes and 20 μL were injected. Flow rate and temperature were set at 20 μL min⁻¹ and 25 °C, respectively. Method validation was performed according to the European Commission Decision 657/2002/EC. Sample detection limits were between 2.8 and 25 μg kg⁻¹, and good linearity was observed up to 250 μg kg⁻¹ for all analytes. Acceptable and constant recoveries of 96% for enrofloxacin, 77% for its metabolite ciprofloxacin, and 64% for flumequine, with RSDs (n = 4) lower than 8%, were obtained at the 100 μg kg⁻¹ maximum level permitted in milk. Recoveries between 70% and 83% were obtained when difloxacin, sarafloxacin and ofloxacin (not allowed in animals that produce milk for human consumption) were added to milk samples at levels in the range 75–150 μg kg⁻¹. Decision limit (CC_α), detection capability (CC_β), repeatability, within-laboratory reproducibility and robustness were compliant with European Union regulations.     

Cadmium levels in food containing crab brown meat: A brief survey from UK retailers

As the brown meat of crabs accumulates cadmium (Cd) to elevated concentrations, the European Commission has recommended consumer advice on the consumption of such seafood products. To supplement available data, 397 samples (including whole crabs and products containing brown crab meat) were collected from UK retailers. Cd concentrations ranged from 0.01 to 26 mg kg −1 wet weight (ww) and mean and median concentrations of 3.4 and 2.8 mg kg⁻¹ were found, respectively. Although there is no regulatory limit for Cd in brown crab meat, mean concentrations were above the permitted maximum of 0.5 mg kg⁻¹ that applies to the white meat component derived from claws and legs. These data will support the UK Food Standards Agency’s risk assessment and management measures regarding the consumption of brown crab meat by UK consumers.     

Development of HPLC-DAD method for determination of neonicotinoids in honey

After the EU banned the use of the neonicotinoids in flowering crops that honeybees might visit, there has been an increased interest in determining the neonicotinoid residues in honeybee products such as honey. The aim of this study was to develop and optimize an HPLC-DAD analytical method with dispersive liquid–liquid microextraction (DLLME) and QuEChERS sample preparation procedures for the simultaneous analysis of seven neonicotinoids (dinotefuran, nitenpyram, thiametoxam, clothianidin, imidacloprid, acetamiprid and thiacloprid) in honey samples. The liquid chromatographic conditions were optimized by Response surface methodology with Box–Behnken design and Derringer's desirability. The optimized method was validated to fulfill the requirements of SANCO/12571/2013 standard for both sample pretreatment procedures providing results for accuracy (73.1–118.3%), repeatability (3.28–10.40%) and within-laboratory reproducibility (6.45–17.70%), limits of detection (1.5–2.5 μg kg⁻¹) and quantification (5.0–10.0 μg kg⁻¹) with the use of matrix-matched calibration to compensate the matrix effects. For the first time 104 honey samples from Vojvodina were analyzed. The presence of thiacloprid, imidacloprid and thiametoxam was found in a small number of samples implicating the usefulness of ongoing control of honey. Residues were confirmed by LC–MS/MS.     

Evaluation of polycyclic aromatic hydrocarbons in Circassian cheese by high-performance liquid chromatography with fluorescence detection

Polycyclic aromatic hydrocarbons (PAH) in traditional/industrial smoked and unsmoked Circassian cheeses available in Turkish markets were analysed using solid-phase extraction, followed by high-performance liquid chromatography (HPLC) with fluorescence detection. Mean levels of a total of 9 PAHs in smoked traditional and industrial Circassian cheeses were 19.6 and 6.73 μg kg⁻¹, while levels in unsmoked traditional and industrial cheeses were 0.77 and 0.49 μg kg⁻¹, respectively. The dominant individual PAHs found were naphthalene and acenaphthene. Benzo[a]pyrene, a marker compound representing carcinogenic PAHs, was found in 90% and 30% of traditional smoked and unsmoked Circassian cheeses, 52% and 24% of industrial smoked and unsmoked cheeses, respectively. Correlation statistical analysis showed that benzo[a]pyrene was a good marker for total 9 PAHs in Circassian cheese samples (r_{B[a]P/sum of 9 PAHs} = 0.816, p < 0.01) as well as the best marker for 5 carcinogenic PAHs (r_{B[a]P/carcinogenic PAHs} = 0.904, p < 0.01). Risk assessment conducted using daily intakes of sum of 9 PAH levels found in both traditional and industrial smoked Circassian cheese samples showed high risk compared with unsmoked cheeses.     

Assessment of hydroxymethylfurfural and furfural in commercial bakery products

A survey was conducted on the presence of hydroxymethylfurfural (HMF) and furfural in bread and bakery products; for this purpose a reliable extraction procedure followed by high performance liquid chromatography (HPLC) was applied. The performance of the method was evaluated in terms of linearity (r always > 0.99); detection limits (0.001 mg L⁻¹ for furfural and 0.006 mg L⁻¹ for HMF); recovery percentages (98.5–100.5% for HMF and 94.9–98.9% for furfural); intraday precision (<4.65%) and interday precision (<7.51%). Two batches of a wide variety of products commercially available were analysed (a total of 88 samples). HMF and furfural levels presented high variability between products and batches of the same product. Cake/pastry samples showed the lowest HMF content (3.0 mg kg⁻¹ fw) while biscuits showed the highest content (7.8 mg kg⁻¹ fw) (p < 0.05). Regarding furfural, bread samples presented the highest furfural content (5.3 mg kg⁻¹ fw) (p < 0.05), cake/pastry and biscuits showed the lowest content (1.9 and 3.0 mg kg⁻¹ fw, respectively). Chocolate containing samples presented higher amounts of furfural (>20 mg kg⁻¹). These results indicate that special attention should be given to furfural content of bread (due to its daily high consumption) and re-evaluation of dietary exposure.     

A fast and effective method of quantitative analysis of VB1, VB2 and VB6 in B-vitamins complex tablets based on three-dimensional fluorescence spectra

Scattering signals and partial overlapping of target peaks usually appear in fluorescence determination. In this study, the improved wavelet moment method was proposed and applied to the quantitative determination of multiple target components in real B-vitamins complex tablets based on three-dimensional (3D) fluorescence spectra. The correlation coefficients (R) were more than 0.9939, and the correlation coefficients of leave-one-out cross-validation (R_LOO-cv) were more than 0.9376. The inter-day and intra-day variations were less than 5.8% and 6.1%, respectively. The recovery ranged from 97.6% to 109.4%. The limits of detection (LODs) and quantification (LOQs) were less than 0.07 μg mL⁻¹ and 0.13 μg mL⁻¹, respectively. All the statistical parameters indicated that the method was stable and reliable. The application to the practical samples confirmed that wavelet moment method effectively extracted the features of target components in 3D spectra and the proposed method could be applied to the analyses of food or other complex samples.