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.     

Determination of catechins in green tea infusions by reduced flow micellar electrokinetic chromatography

A sulfated-β-cyclodextrin (s-β-CD) modified reduced flow micellar electrokinetic chromatography (RF-MEKC) method was developed and validated for the determination of catechins in green tea. The optimal electrolyte consisted of 0.2% triethylamine, 50 mmol/L SDS and 0.8% s-β-CD (pH = 2.9), allowing baseline separation of five catechins in 4 min. The samples and standards were injected at 0.6 psi for 5 s under constant voltage of −30 kV. Sample preparation simply involved extraction of 2 g of tea with 200 mL water at 95 °C under constant stirring for 5 min. The method demonstrated excellent performance, with limits of detection (LOD) and quantification (LOQ) of 0.02–0.1 and 0.1–0.5 μg/mL, respectively, and recovery percentages of 94–101%. The method was applied to six samples of Brazilian green tea infusions. Epigallocatechin gallate (23.4–112.4 μg/mL) was the major component, followed by epigallocatechin (18.4–78.9 μg/mL), epicatechin gallate (5.6–29.6 μg/mL), epicatechin (4.6–14.5 μg/mL) and catechin (3.2–8.2 μg/mL).     

Distribution of fungi and aflatoxins in a stored peanut variety

The objective of the present study was to evaluate the mycoflora and occurrence of aflatoxins in stored peanut samples (hulls and kernels) from Tupã, State of São Paulo, Brazil. The samples were analyzed monthly over a period of one year. The results showed a predominance of Fusarium spp. (67.7% in hulls and 25.8% in kernels) and Aspergillus spp. (10.3% in hulls and 21.8% in kernels), and the presence of five other genera. The growth of Aspergillus flavus was mainly influenced by temperature and relative humidity. Analysis of hulls showed that 6.7% of the samples were contaminated with AFB₁ (mean levels = 15–23.9 μg/kg) and AFB₂ (mean levels = 3.3–5.6 μg/kg); in kernels, 33.3% of the samples were contaminated with AFB₁ (mean levels = 7.0–116 μg/kg) and 28.3% were contaminated with AFB₂ (mean levels = 3.3–45.5 μg/kg). Analysis of the toxigenic potential revealed that 93.8% of the A. flavus strains isolated were producers of AFB₁ and AFB₂.     

Inactivation of Geobacillus stearothermophilus in canned food and coconut milk samples by addition of enterocin AS-48

The cyclic bacteriocin enterocin AS-48 was tested on a cocktail of two Geobacillus stearothermophilus strains in canned food samples (corn and peas), and in coconut milk. AS-48 (7 μg/g) reduced viable cell counts below detection levels in samples from canned corn and peas stored at 45 °C for 30 days. In coconut milk, bacterial inactivation by AS-48 (1.75 μg/ml) was even faster. In all canned food and drink samples inoculated with intact G. stearothermophilus endospores, bacteriocin addition (1.75 μg per g or ml of food sample) rapidly reduced viable cell counts below detection levels and avoided regrowth during storage. After a short-time bacteriocin treatment of endospores, trypsin addition markedly increased G. stearothermophilus survival, supporting the effect of residual bacteriocin on the observed loss of viability for endospores. Results from this study support the potential of enterocin AS-48 as a biopreservative against G. stearothermophilus.     

Development and validation of an HPLC-method for determination of free and bound phenolic acids in cereals after solid-phase extraction

Whole cereal grains are a good source of phenolic acids associated with reduced risk of chronic diseases. This paper reports the development and validation of a high-performance liquid chromatography–diode array detection (HPLC–DAD) method for the determination of phenolic acids in cereals in either free or bound form. Extraction of free phenolic acids and clean-up was performed by an optimised solid-phase extraction (SPE) protocol on Oasis HLB cartridges using aqueous methanol as eluant. The mean recovery of analytes ranged between 84% and 106%. Bound phenolic acids were extracted using alkaline hydrolysis with mean recoveries of 80–95%, except for gallic acid, caffeic acid and protocatechuic acid. Both free and bound phenolic extracts were separated on a Nucleosil 100 C₁₈ column, 5 μm (250 mm × 4.6 mm) thermostated at 30 °C, using a linear gradient elution system consisting of 1% (v/v) acetic acid in methanol. Method validation was performed by means of linearity, accuracy, intra-day and inter-day precision and sensitivity. Detection limits ranged between 0.13 and 0.18 μg/g. The method was applied to the analysis of free and bound phenolic acids contents in durum wheat, bread wheat, barley, oat, rice, rye, corn and triticale.     

Simple and high-throughput method for the multimycotoxin analysis in cereals and related foods by ultra-high performance liquid chromatography/tandem mass spectrometry

A rapid, reliable and sensitive method was developed to determine 12 mycotoxins (deoxynivalenol, aflatoxins B1, B2, G1, G2 and M1, fumonisins B1 and B2, ochratoxin A, HT-2 and T-2 toxin and zearalenone) simultaneously in maize, walnuts, biscuits and breakfast cereals. The method is based on a single extraction step using acetonitrile/water mixture (80/20 v/v) followed by ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC–MS/MS). The selectivity of the MS/MS detection allowed the elimination of further clean up steps. Extraction, chromatographic and detection conditions were optimised in order to increase sample throughput and sensitivity. Matrix-matched calibration was used for quantification and recoveries of the extraction process ranged from 70.0% and 108.4%, with relative standard deviations lower than 25% in all the cases, when samples were fortified at 5 and 50 μg/kg. Limits of detection ranged from 0.01 to 2.1 μg/kg and limits of quantification ranged from 0.03 to 6.30 μg/kg, which were always below the tolerance levels of mycotoxins set by European Union in the matrices evaluated. Several samples were analysed and aflatoxins B1, B2, G1, G2 and T-2 toxin were detected in one maize sample, with concentrations lower than 6.0 μg/kg and deoxynivalenol was detected in a breakfast cereal at 42.1 μg/kg.     

Antioxidant activity and phenolic content of 16 raisin grape (Vitis vinifera L.) cultivars and selections

Six raisin grape cultivars and 10 new raisin grape selections were analyzed for antioxidant activity (ABTS assay) and for total and individual phenolic compounds. Samples were freeze–dried and values are reported on a dry weight basis. Antioxidant activity across the 16 samples ranged from 7.7 to 60.9 μmol Trolox/g DW, with A95-27 exhibiting the greatest activity. Total phenolic content, determined in gallic acid equivalents using the Folin–Ciocalteau assay, ranged from 316.3 to 1141.3 mg gallic acid/100 g DW and was strongly correlated (r = 0.990) with antioxidant results. Concentrations of individual phenolics were determined by HPLC. trans-Caftaric acid was the predominant compound in all samples. A95-15 contained the lowest concentration (153.5 μg/g DW) of caftaric acid, while Fiesta contained the highest concentration (598.7 μg/g DW). Selections A56-66, A95-15, and A95-27 had much higher levels of catechin (86.5–209.1 μg/g DW) and epicatechin (126.5–365.7 μg/g DW) than the other samples.     

Occurrence of deoxynivalenol and T-2 toxin in bread and pasta commercialised in Spain

Deoxynivalenol and T-2 toxin were extracted from wheat-based bread (n = 75) and pasta (n = 75) samples using a mixture of acetonitrile:water (86:14 v/v); for analysis, gas chromatography/mass spectrometry after derivatisation with trifluoroacetic anhydride was utilised. The recovery of deoxynivalenol and T-2 toxin from both food matrixes ranged from 90.1 to 94.0%. The occurrence of these mycotoxins in bread was 28.0% and 2.6% for deoxynivalenol and T-2 toxin, respectively, whereas in pasta, the occurrence of both mycotoxins was higher, varying from 9.3 to 62.7%. The mean content of deoxynivalenol (42.5 μg/kg) in bread was lower than the content of T-2 toxin (68.37 μg/kg), while in pasta the content of deoxynivalenol (137.1 μg/kg) was superior. The estimated daily intake of deoxynivalenol and T-2 toxin from the consumption of these products represents 8.4% and 0.2% of the tolerable daily intake, respectively. These results back up the necessity to take a vigilant attitude in order to prevent human intake of trichothecenes. This information is necessary and of high priority in order to protect the consumer’s health from the risk of exposure to these toxins.     

Monitoring and risk assessment of pesticide residues in yuza fruits (Citrus junos Sieb. ex Tanaka) and yuza tea samples produced in Korea

The objective of this study was to establish an analytical method to measure pesticides used to cultivate yuza (Citrus junos Sieb. ex Tanaka) and to analyze pesticide residue levels of yuza and yuza tea samples. Risk assessments were also performed by calculating estimated daily intake (EDI) and acceptable daily intake (ADI). An excellent linear correlation was achieved with coefficient correlation values of 0.9750–0.9999. Percent recoveries were 80.4–109.9% for most pesticides with a <6.9% relative standard deviation (RSD). The limits of quantification for the method were 0.10–0.67 μg/ml. The RSD of intra-day and inter-day variability was <15.3%. Seven pesticides in yuza (n = 80) and yuza tea (n = 75) were analyzed with the optimized analytical method. Acequinocyl, spirodiclofen and carbendazim were detected in yuza samples in the concentration range of 0.07–0.15 μg/g, 0.11–1.89 μg/g, and 0.03–5.15 μg /g, respectively, whereas chlorpyrifos, prothiofos, phosalone, and deltamethrin were not detected in yuza or yuza tea. The concentrations of acequinocyl, spirodiclofen and carbendazim ranged from 0.18–1.05 μg/g, 0.13–0.29 μg/g, and 0.17–2.36 μg/g, respectively, in yuza tea samples. The percent ratios of EDI to ADI for acequinocyl, spirodiclofen, and carbendazim were 24.6%, 22.7%, and 58.5%, respectively.     

Sterigmatocystin presence in typical Latvian grains

Ninety five samples of different Latvian grains (wheat, buckwheat, barley, oats and rye) from the year 2006 and 120 samples from the year 2007 were analyzed for Aspergillus ssp. mycotoxin–sterigmatocystin (STC) content. 13.7% of the analyzed 2006 year samples were positive for STC with the concentration levels ranging from <0.7 to 83 μg/kg and 35% of the analyzed 2007 year samples were positive for STC with the concentration levels ranging from <1 to 47 μg/kg. A previously developed sensitive LC – Electrospray Positive Ionization – MS/MS method was applied for the analysis of STC in grains. Method includes sample extraction with acetonitrile/water solution, solid phase extraction (SPE) on Strata X SPE column, separation on reversed phase C₁₈ column and STC detection by LC–MS/MS.     

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.     

Development and validation of a new LC–MS/MS method for the simultaneous determination of six major ergot alkaloids and their corresponding epimers. Application to some food and feed commodities

A liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for the simultaneous determination of six major ergot alkaloids, ergometrine, ergosine, ergotamine, ergocornine, ergokryptine and ergocristine, as well as their corresponding epimers in food and feed samples. The method involves extraction under alkaline conditions and subsequent clean-up by applying a simple and rapid liquid–liquid partitioning procedure prior to LC–MS/MS analysis. Evaluation of the method revealed good linearity, accuracy and precision. The limits of quantification varied from 0.1 to 1 μg/kg depending on the analyte and matrix. The average extraction and clean-up recoveries in different matrices were between 45 (only for ergometrine in biscuit) and 90%. The uncertainty associated with the analytical method was not higher than 51% and 30%, at concentration levels of 2.5 and 150 μg/kg respectively. Analyte epimerization proved to be minimal during the analytical procedure. The method has been successfully applied to the determination of ergot alkaloids in some Belgian food and feed commodities. Ergot alkaloids were found in 104 out of 122 samples investigated. Ergosine was the most frequently occurring alkaloid, while the highest levels were observed for ergotamine, ergocristine or ergosine, depending on the product type. The total alkaloid content in positive samples varied from 1 to 1145 μg/kg.     

Co-occurrence of mycotoxins in corn samples from the Northern region of Paraná State,Brazil

Natural mycoflora and co-occurrence of fumonisins and aflatoxins were evaluated in 300 freshly-harvested corn samples (2003 and 2004 crops) collected at two points of the production chain in the Northern region of Paraná State, Brazil. In the 2003 crop, fumonisins were detected in 100% of samples and the mean levels were 2.54 μg/g in the reception and 3.12 μg/g in the pre-drying samples. On the other hand, in the 2004 crop fumonisins were detected in 98.9% and 95% of the reception and pre-drying samples, respectively. The mean levels were 1.31 μg/g in the reception, and 1.36 μg/g in the pre-drying samples. Aflatoxins were not detected in 92% of the samples analysed. The maximum probable daily intake (PDI_M) estimated for the Brazilian population (0.95 μg/kg body weight/day) is below the tolerable daily intake of 2.0 μg/kg body weight/day for fumonisin B₁.     

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.     

Rhus verniciflua Stokes flavonoid extracts have anti-oxidant,anti-microbial and α-glucosidase inhibitory effect

We isolated four compounds, fustin, gallic acid, 3′,4′,7-trihydroxyflavone, and fisetin from Rhus verniciflua. These compounds showed electron donation ability (87–94%) that was stronger than butylated hydroxyanisole (52%). Gallic acid (OD₇₀₀ = 1.98) showed the highest reducing power, and the other isolated compounds (OD₇₀₀ = 0.66–1.31) showed stronger activity than α-tocopherol (OD₇₀₀ = 0.21). The ethyl-acetate fraction had the highest phenolic content (723 mg GAE/g), followed by the 80% ethanolic extract (597 mg GAE/g). For Gram-negative bacteria, fisetin had the most potent anti-bacterial activity (MIC = 8 μg/ml) against Escherichia coli. 3′,4′,7-Trihydroxyflavone (106%), the 80% ethanolic extract (101%), and ethyl-acetate (98%) had the most powerful α-glucosidase inhibitory effect at 50 μg/ml. R. verniciflua extracts have potential as functional food additives.     

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.     

Exploration of Vanilla pompona from the Peruvian Amazon as a potential source of vanilla essence: Quantification of phenolics by HPLC-DAD

This study provides the first chemical investigation of wild-harvested fruits of Vanilla pompona ssp. grandiflora (Lindl.) Soto-Arenas developed in their natural habitat in the Peruvian Amazon. Flowers were hand-pollinated and the resulting fruits were analysed at different developmental stages using an HPLC-DAD method validated for the quantification of glucovanillin and seven other compounds. The method showed satisfactory linearity (r² > 0.9969), precision (coefficient of variation <2%), recoveries (70–100%), limit of detection (0.008–0.212 μg/ml), and limit of quantification (0.027–0.707 μg/ml). The evaluation of crude and enzyme-hydrolyzed Soxhlet-extracted samples confirmed the leading role of glucosides in fruit development. LC–ESI-MS studies corroborated the identities of four glucosides and seven aglycones, among them vanillin (5.7/100 g), 4-hydroxybenzyl alcohol (3.6/100 g), and anisyl alcohol (7.1/100 g) were found in high concentrations. The attractive flavor/aroma profile exhibited by wild V. pompona fruits supports studies focused on the development of this species as a specialty crop.     

Deoxynivalenol and nivalenol in commercial wheat grain related to Fusarium head blight epidemics in southern Brazil

A three-year (2006-2008) survey on commercial wheat grain was conducted aimed at quantifying the intensity of Fusarium head blight epidemics related to kernel quality and levels of deoxynivalenol (DON) and nivalenol (NIV). Grain samples, obtained from 38 municipalities throughout the state of Rio Grande do Sul, Brazil, were assessed visually for Fusarium-damaged kernels (FDK) and chemically using liquid chromatography-mass spectrometry (LC-MS/MS). Overall FDK mean levels were 15.5%, not differing among the years. Co-contamination was predominant (59/66) across samples and overall mean levels of DON and NIV were 540 and 337 μg/kg, respectively. When the levels of both mycotoxins were added together (DON + NIV), a higher correlation with FDK was found (R = 0.36, P < 0.01), compared to single toxin data. For the first time, the presence of NIV in levels comparable to DON is reported from a multi-year regional epidemiological survey in the country which should be of concern to the small grains industry.     

Effect of canned tuna fish processing steps on lead and cadmium contents of Iranian tuna fish

The contents of Pb and Cd in two species of Iranian tuna fish (yellowfin and skipjack), which were caught from the Persian Gulf and Oman Sea, and the effects of canning processing steps on their contents were assessed by electrothermal atomic absorption spectrometry. The results revealed that the levels of lead and cadmium throughout the processing steps in yellowfin were in range of 0.154 ± 0.019–0.441 ± 0.025 μg/g and 0.029 ± 0.002–0.084 ± 0.0005 μg/g, respectively. Pb and Cd concentrations from received fish to final product in skipjack were found to be in range of 0.072 ± 0.031–0.218 ± 0.031 μg/g and 0.016 ± 0.001–0.062 ± 0.002 μg/g, respectively. The limit of detection for lead and cadmium were 0.058 μg/g (11.6022 μg/l) and 0.0007 μg/g (0.1485 μg/l), respectively. Results from paired sample t-test analysis showed that defrosting, cooking, and sterilisation by autoclave would reduce the contents of lead and cadmium, considerably.     

Determination of biogenic amines in foods using ultra-performance liquid chromatography (UPLC)

A rapid ultra-performance liquid chromatographic (UPLC) method for the determination of biogenic amines (putrescine, cadaverine, spermidine, spermine, phenylethylamine, histamine, tyramine and tryptamine) in selected food samples is described. The eight biogenic amines, which are the most important to be determined in food samples, were derivatized with dansyl chloride prior to UPLC separation. The dansylated amines were separated on an Agilent Zorbax Eclipse XDB – C18 column (50 × 4.6 mm ID, 1.8 μm) using gradient elution with a binary system of acetonitrile–water, a flow rate of 1.0 ml/min and UV detection at 225 nm. The analysis is very fast, all amines are well resolved and are eluted from the column in less than 6 min. The average repeatability of the method ranged between 1.02% and 2.14%. Limits of detection (LODs) for considered amines ranged between 0.032 and 0.098 μg/l; calibration curves showed very good linearity (r = 0.9994–1.0000). The method was applied to the analysis of amines in pork, beef, chicken and fish meat, cheese and edible mushrooms.