Occurrence of furan in commercial processed foods in Brazil

Selected commercial processed foods available in the Brazilian market (306 samples) were analysed for furan content using a validated gas chromatography-mass spectrometry method preceded by headspace solid phase micro-extraction (HS-SPME-GC/MS). Canned and jarred foods, including vegetable, meat, fruit and sweet products, showed levels up to 32.8?µg?kg^?1, with the highest concentrations observed in vegetables and meats. For coffee, furan content ranged from 253.0 to 5021.4?µg?kg^?1 in the roasted ground coffee and from not detected to 156.6?µg?kg^?1 in the beverage. For sauces, levels up to 138.1?µg?kg^?1 were found. In cereal-based products, the highest concentrations (up to 191.3?µg?kg^?1) were observed in breakfast cereal (corn flakes), cracker (cream crackers) and biscuit (wafer). In general, these results are comparable with those reported in other countries and will be useful for a preliminary estimate of the furan dietary intake in Brazil.     

Determination of furan levels in commercial samples of baby food from Brazil and preliminary risk assessment

Commercial baby food samples available on the Brazilian market (n = 31) were analysed for furan content using a gas chromatography-mass spectrometry method preceded by solid-phase microextraction. A limit of detection of 0.7 µg kg^?1, a limit of quantitation of 2.4 µg kg^?1, mean recoveries varying from 80% to 107%, and coefficients of variation ranging from 5.6% to 9.4% for repeatability and from 7.4% to 12.4% for within-laboratory reproducibility were obtained during an in-house validation. The levels of furan found in the samples were from not detected to 95.5 µg kg^?1. Samples containing vegetables and meat showed higher furan levels as compared with those containing only fruits. An exposure assessment showed furan intakes up to 2.4 µg kg^?1 body weight day^?1 (99th percentile) for babies fed exclusively with commercial baby foods. Margins of exposure obtained from intakes estimated in this work indicated a potential public health concern.     

Furan in the baby-food samples purchased from the Finnish markets – Determination with SPME–GC–MS

A method applying solid-phase microextraction followed by gas chromatography–mass spectrometric determination was in-house validated and used to study furan concentrations in baby-food samples purchased from the Finnish markets. The validation parameters showed that the method was well applicable for the reliable analysis of furan. Furan was analysed in 21 different baby-food samples as three independent replicates. The mean levels of furan varied between 4.7 and 90.3 μg kg⁻¹ being well in accordance with the levels reported in other studies. The mean concentrations of similar product formulas based on their ingredients were 9.2, 37.0 and 49.6 μg kg⁻¹ for fruit-, vegetables- and meat-containing baby-foods, respectively. According to the statistical analyses, fruit-based baby-food samples had significantly lower concentrations of furan as compared to other formulas. Based on our exercise, it seems that a low margin of safety exists between the extreme worst case infant exposures and the deduced NOAEL of furan on experimental animals, particularly for a clear rodent carcinogen.     

Furan in commercial baby foods from the Spanish market: estimation of daily intake and risk assessment

ABSTRACT

The occurrence of furan in commercial baby food samples from the Spanish market was evaluated using an automated headspace solid-phase microextraction method coupled to gas chromatography-mass spectrometry (HS-SPME-GC-MS). A total of 76 baby food samples including infant formula, baby cereals, fruit in cans and/or jars, vegetables, meat, and fish, were surveyed for furan content. The lowest concentration of this compound was found in infant formula (<0.02–0.33 ng ml^?1), and cereal-based food (0.15–2.1 ng g^?1) while baby food containing fish showed the highest concentrations (19–84 ng g^?1). Following recommendation of the European Food Safety Authority (EFSA), the effect on furan content was evaluated of consumer home preparation of foods, heating and handling. Furan concentrations were reduced by up to 35% when samples were heated in a dish using microwave oven and by up to 53% when a hot water bath was used. Finally, we estimated the furan intake from baby food consumption (0.002–1.18 µg kg^?1 body weight day^?1) and we calculated the margin of exposure (MOE) from samples as purchased and also after home preparation of the food. For infant formula and cereal baby foods, the MOEs (26,278–412,776) indicated no infant health concern or priority, while for meat and fish-based baby foods the values pointed to a potential public health risk, even considering the furan losses during preparation at home.     

Are Chileans exposed to dietary furan?

Chilean consumer preferences include foods that may contain considerable amounts of furan, a potential human carcinogen. However, there is no information regarding dietary exposure to furan in Chile. Thus, the objective of this work was to determine the Chilean exposure to dietary furan. To accomplish this objective, the furan concentration of 14 types of commercial foods processed at high temperature were analysed based on a modified headspace-GC/MS (HS-GC/MS) method in which the limits of detection for different food matrices ranged from 0.01 to 0.6 ng g^?1. In addition, a risk assessment was made with exposure estimates based on dietary data from national studies on different age groups (9-month-old babies, school children, adults and elderly people). Of the food items surveyed “American”-type coffee (espresso coffee plus hot water) obtained from automatic coffee machine (936 ng g^?1) and low moisture starchy products like crisps and “soda”-type crackers showed the highest furan concentrations (259 and 91 ng g^?1, respectively). Furthermore, furan was also found in samples of breakfast cereals (approximately 20 ng g^?1), jarred fruit baby foods (8.5 ng g^?1) and orange juice (7.0 ng g^?1). School children (aged 9–13 years) represented the highest intake of furan (about 500 ng kg^?1_bw day^?1), with margins of exposure of 2479 and 2411, respectively, which points to a possible public health risk.     

Determination and surveillance of hydrocortisone and progesterone in livestock products by liquid chromatography-tandem mass spectrometry

A simple analytical method for the determination of hydrocortisone and progesterone in bovine, swine, and chicken muscle and eggs was developed. Hydrocortisone and progesterone were extracted with acetonitrile and subsequently cleaned-up using an Oasis^® HLB mini-cartridge. The method was validated in accordance with Japanese guidelines and exhibited trueness from 86.6% to 104.3% and precision (relative standard deviations (RSDs) of repeatability and within reproducibility were under 8.7% and 11.7%, respectively). The method was applied to 103 bovine muscle, 137 swine muscle, 69 chicken muscle and 52 egg samples that were commercially available in Tokyo, Japan. The hydrocortisone concentration was 0.9–41.2 µg kg^?1 in all bovine muscle samples, with an average of 7.7 µg kg^?1 and a median of 6.2 µg kg^?1. The progesterone concentration in 50 samples exceeded the limit of quantification (LOQ) and reached a maximum of 95.4 µg kg^?1. Hydrocortisone was also detected in all swine muscle samples at concentrations of 2.0–56.0 µg kg^?1. Its average and median concentrations amounted to 13.1 and 11.3 µg kg^?1, respectively. Twenty-three samples contained progesterone levels surpassing the LOQ, with a maximum concentration of 107.0 µg kg^?1. No chicken muscle samples contained any of the analytes. The progesterone concentration was 15.5–200.0 µg kg^?1 in all egg samples, with an average of 95.4 µg kg^?1 and a median of 90.5 µg kg^?1.     

Feed additives diclazuril and nicarbazin in egg and liver samples from Croatian farms

In total 307 egg and 275 liver samples were examined for nicarbazin and 365 eggs for diclazuril over a 30-month period. Enzyme-linked immunosorbent assay methods used for quantification were validated according to European Commission Decision 2002/657/EC. Non-compliant samples were confirmed by LC-MS/MS. Mean diclazuril concentrations in egg samples were 0.31?µg?kg^?1, which is below the MRL. In only one egg sample, 2.26?µg?kg^?1 was determined by enzyme-linked immunosorbent assay, although confirmation by LC-MS/MS gave a value of 1.6?µg?kg^?1. Mean nicarbazin levels determined were 1.85?µg?kg^?1 in egg and 21.1?µg?kg^?1 in liver samples. Four samples, one egg and three livers, yielded elevated concentrations of nicarbazin, but only in the egg sample the LC-MS/MS method confirmed nicarbazin (106?µg?kg^?1) above the MRL value.     

Survey of aflatoxins in maize tortillas from Mexico City

In Mexico, maize tortillas are consumed on a daily basis, leading to possible aflatoxin exposure. In a survey of 396 2-kg samples, taken over four sampling days in 2006 and 2007 from tortilla shops and supermarkets in Mexico City, aflatoxin levels were quantified by HPLC. In Mexico, the regulatory limit is 12?µg?kg^?1 total aflatoxins for maize tortillas. In this survey, 17% of tortillas contained aflatoxins at levels of 3–385?µg?kg^?1 or values below the limit of quantification (<LOQ) and, of these, 13% were >12?µg?kg^?1 and 87% were below the regulatory limit. Average aflatoxin concentrations in 56 contaminated samples were: AFB₁ (12.1?µg?kg^?1); AFB₂ (2.7?µg?kg^?1); AFG₁ (64.1?µg?kg^?1) and AFG₂ (3.7?µg?kg^?1), and total AF (20.3?µg?kg^?1).     

Development of an analytical method and survey of foods for furan, 2-methylfuran and 3-methylfuran with estimated exposure

Furan has been found to form in foods during thermal processing. These findings, a classification of furan as a possibly carcinogenic to humans, and a limited amount of data on the concentration of furan in products on the Canadian market prompted the authors to conduct a survey of canned and jarred food products. Methyl analogues of furan, 2-methylfuran and 3-methylfuran, were analysed concurrently with furan via a newly developed isotope dilution method, as these analogues were detected in foods in the authors’ earlier work and are likely to undergo a similar metabolic fate as furan itself. The paper reports data on 176 samples, including 17 samples of baby food. The vast majority of samples were packaged in cans or jars. Furan was detected above 1 ng g^?1 in all non-baby food samples with a median of 28 ng g^?1 and concentrations ranging from 1.1 to 1230 ng g^?1. Also, 96% of these samples were found to contain 2-methylfuran above 1 ng g^?1 with a median of 12.8 ng g^?1 and a maximum concentration of 152 ng g^?1, while 81% of samples were found to contain 3-methylfuran above 1 ng g^?1 with a median of 6 ng g^?1 and a maximum concentration of 151 ng g^?1. Similarly, furan was detected above 1 ng g^?1 in all baby food samples with a median of 66.2 ng g^?1 and concentrations ranging from 8.5 to 331 ng g^?1. Also, 100% of these samples were found to contain 2-methylfuran above 1 ng g^?1 with a median of 8.7 ng g^?1 and a maximum concentration of 50.2 ng g^?1, while 65% of samples were found to contain 3-methylfuran above 1 ng g^?1 with a median of 1.6 ng g^?1 and a maximum concentration of 22.9 ng g^?1. Additionally, three coffee samples were analysed ‘as is’, without brewing, and were found to have high levels of furans, especially 2-methylfuran, at a maximum of 8680 ng g^?1. Using this data set, dietary exposures to furan and total furans were calculated. Average furan and total furan intakes by adults (≥20 years) were estimated at approximately 0.37 and 0.71 µg kg^?1 of body weight day^?1 respectively.     

Evaluation of acrylamide and selected parameters in some Turkish coffee brands from the Turkish market

The purpose of this study was to measure acrylamide (AA) levels and selected parameters of different traditional Turkish coffees. AA, 5-hydroxymethylfurfural (HMF), total reducing sugar, protein, pH, moisture, dry matter (DM) as well as ash, caffeine and soluble solids content (SSC) in DM, L*, a*, b* colour parameters of coffee samples were determined and the correlation between AA level and these parameters were investigated. A total of 36 coffee samples (20 Turkish, 8 Dibek and 8 Terebinth coffee) from the Turkish market were examined. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was validated for the detection and quantitation of AA in coffee samples. The calibration curve was linear (R² ≥ 0.999) over the range of 30–1000 μg kg^?1. The limit of detection (LOD) and limit of quantification (LOQ) were found as 4.6 μg kg^?1 and 15.5 μg kg^?1, respectively. The amounts of AA in analysed coffee samples were in the range 31.1 ± 0.6 to 323.4 ± 5.4 µg kg^?1. The highest mean AA levels were found in Terebinth coffees (240.3 μg kg^?1) followed by Turkish coffees (204.3 µg kg^?1) and then Dibek coffees (78.6 µg kg^?1). No tested Turkish coffee samples had an AA concentration above the indicative value (450 µg kg^?1) for roast coffee recommended by the European Commission (EC) in 2011. In addition, a strong positive correlation was found between HMF values and AA amounts of selected coffee types.     

Survey of fumonisins B1, B2 and B3 in conventional and organic retail corn products in Spain and Italy and estimated dietary exposure

A survey was conducted to determine the occurrence of fumonisin B₁, B₂ and B₃ during 2007 in 186 samples of organic and conventional locally available corn products. Samples included baby food (n = 62), corn flour (11), cornflakes (23), pasta (14), cookies (17) and other corn products (59) were obtained from popular markets of Valencia (Spain) and Perugia (Italy). The analytical method used pressurized liquid extraction and liquid chromatography/electrospray ionization tandem mass spectrometry with a triple quadrupole (QqQ) analyser. Of the 104 Spanish samples, 22% contained levels in the range of 2–449 µg kg^?1, 2–229 µg kg^?1 and 6–105 µg kg^?1 for FB₁, FB₂ and FB₃, respectively, while 19 (23%) of the 82 Italian samples were positive with quantifiable levels between 2–235 µg kg^?1, 3–187 µg kg^?1, and 4–40 µg kg^?1 for fumonisins B₁, B₂ and B₃, respectively. Overall, none of the Italian samples and only one organic baby food sample from a Spanish market was above the maximum permitted levels established by European legislation. Fumonisins were found mostly in corn flour followed by cookies and cornflakes. Eleven samples from Spain and nine samples from Italy were organic products, being contaminated the 72% and 77% of the samples, respectively. Analysis of the results showed that levels of fumonisins in corn products were similar in Italy and Spain. The safety of fumonisin intake through corn products was demonstrated by the calculation of the estimated daily intake of both populations considering organic and conventional products separately, which ranged from 1.7 × 10^?3 to 0.72 µg kg^?1 bw day^?1 and comparing them with the provisional maximum total daily intake (PMTDI) of 2 µg kg^?1 bw day^?1 established by the European Union.     

Survey of acrylamide levels in Chinese foods

A survey of levels of acrylamide (AA) in 349 food products obtained from the Chinese market was conducted. AA was determined by an liquid chromatography-tandem mass spectrometry (LC-MS/MS) method. The limit of detection (LOD) and the limit of quantification (LOQ) of the method in four different matrices ranged from 0.8 to 10 µg kg^?1 and from 4.0 to 25 µg kg^?1, respectively. The results from this survey indicated that AA was present in all samples except drinking water and tea. AA contents in different samples varied greatly according to the raw materials and processing conditions. The highest level of AA was found in potato products, with an average level of 1467 µg kg^?1. Preliminary estimates of AA exposure and risk assessment of AA from foods in the Chinese population were performed using a combination of data obtained in the present survey and 2002 dietary consumption survey carried out in 2002 for the Chinese population. The average dietary exposure of AA was estimated to be 0.38 µg kg^?1 body weight day^?1, which is relatively low compared with the result reported by the Food and Agricultural Organization/World Health Organization (FAO/WHO). Furthermore, the margin of exposure for neurotoxicity, reproductive toxicity, and carcinogenicity of AA was calculated to be 1318, 5250, and 787, respectively.     

Occurrence of ochratoxin A and citrinin in Czech cereals and comparison of two HPLC methods for ochratoxin A detection

The aims of the study were to obtain information about the occurrence of ochratoxin A (OTA) and citrinin (CIT) in cereals harvested in the Czech Republic and to compare two analytical procedures for detecting OTA. A total of 34 cereal samples, including two matrix reference materials (R-Biopharm, Germany), were analysed. The results were compared with the limit for raw cereal grains used as a foodstuff according to Commission Regulation No. 1881/2006, which allows a maximum OTA level of 5 µg kg^?1. Compared were two methods based on the high-performance liquid chromatography principle, one using the immunoaffinity columns OchraTest? (VICAM) and the second based on solvent partition (PART), both followed by fluorescence detection. The highest OTA contents were found in two barley samples. According to the method employed, the results for the first sample (malting barley) were VICAM = 31.43 µg kg^?1 and PART = 44.74 µg kg^?1. For the second sample (feeding barley) they were VICAM = 48.63 µg kg^?1 and PART = 34.40 µg kg^?1. Two samples of bread wheat had an OTA content approaching the legal limit (VICAM = 4.71 µg kg^?1 and PART = 6.03 µg kg^?1; VICAM = 4.12 µg kg^?1 and PART = 3.95 µg kg^?1). CIT was analysed using the PART method only, and its highest content (93.64 µg kg^?1) was found for the malting barley sample with high OTA content (44.74 µg kg^?1 as analysed using PART).     

Migration of bisphenol A from polycarbonate baby bottles under real use conditions

Migration of the potential endocrine disrupter, bisphenol A (BPA), from 31 polycarbonate (PC) baby bottles into aqueous food simulants was studied under real repetitive use, using a sensitive and fully validated liquid chromatographic method with fluorescence detection. Confirmation of the presence of BPA was performed by liquid chromatography–mass spectrometry (LC–MS). The effects of cleaning in a dishwasher or with a brush, sterilization with boiling water and the temperature of migration were examined. It was shown that temperature was the crucial factor for the migration of BPA from the plastic bottles to water. All samples released BPA in the concentration range 2.4–14.3 µg kg^?1 when filled with boiled water and left at ambient temperature for 45 min. The decrease of BPA release in the sterilization water and in the food simulant over 12 cycles of use indicated that the hypothesis of polymer degradation in water is dubious. Estimated infantile dietary exposure, regarding the use of PC baby bottles, ranged between 0.2 and 2.2 µg kg^?1 bw day^?1, which is below the Tolerable Daily Intake of 50 µg kg^?1 bw recently established by EFSA.     

Occurrence and intake of deoxynivalenol in cereal-based products marketed in Korea during 2007–2008

The occurrence of deoxynivalenol (DON) was investigated in 514 cereal-based products (corn-based, n = 125; barley-based, n = 96; wheat-based, n = 94; rice-based, n = 199) marketed in Korea during 2007?2008, and estimates of DON intake were determined. Samples were analysed by high-performance liquid chromatography (HPLC) with ultraviolet light (UV) detection after immunoaffinity clean-up. The limits of detection (LOD) and limits of quantification (LOQ) were 2.2 and 5.6 µg kg^–1, respectively. Recoveries and repeatability expressed as coefficients of variation (CV) were 82.3–100% and 2.4–15.3% in beer, bread and dried corn. The incidences and mean levels of DON were 56% and 68.9 µg kg^?1 for corn-based products, 49% and 24.1 µg kg^?1 for wheat-based products, 43% and 7.5 µg kg^?1 for barley-based products, and 16% and 3.4 µg kg^?1 for rice-based products, respectively. The estimated daily intake of DON from the consumption of rice-based, wheat-based, barley-based and corn-based products were 0.0038 µg kg^?1 bw day^?1, 0.0032 µg kg^?1 bw day^?1, 0.0015 µg kg^?1 bw day^?1 and 0.0002 µg kg^?1 bw day^?1, respectively. These values represent 0.38%, 0.32%, 0.25% and 0.01% of the provisional maximum tolerable daily intake (PMTDI) of 1 µg kg^?1 bw day^?1. These results indicate that rice-based products are major contributors to DON exposure in Korea, even though the current exposure level is unlikely to cause adverse health effects.     

Simultaneous determination of type A,B and D trichothecenes and their occurrence in cereals and cereal products

A sensitive LC–MS/MS method for the simultaneous determination of type A, B and D trichothecenes in cereals is presented. The limits of detection ranged between 0.1 and 0.7 µg kg^?1 for all analytes. The method was applied to 289 representatively drawn samples of wheat, rye and oat products. Ninety-four percent of the wheat samples (n = 130), 95% of the rye samples (n = 61) and 100% of the oat samples (n = 98) were contaminated with the type A trichothecenes T-2 and HT-2 toxin. Median levels of T-2/HT-2 (sum of the toxins) were 0.91, 0.53 and 8.2 µg kg^?1, respectively. Highest levels were found in wheat bran (24 µg kg^?1), rye kernels (3.1 µg kg^?1) and oat flakes (85 µg kg^?1). All wheat and rye samples and 75% of the oat samples were contaminated with the type B trichothecene deoxynivalenol. Median levels of this toxin were 23, 15 and 0.53 µg kg^?1, respectively. Highest levels were found in wheat bran (1160 µg kg^?1), rye kernels (288 µg kg^?1) and oat flakes (55 µg kg^?1). The type B trichothecene nivalenol was detected in 67% of the wheat samples, in 3% of the rye samples and in 24% of the oat samples with highest levels in wheat bran (96 µg kg^?1), rye kernels (1.8 µg kg^?1) and in oat flakes (17 µg kg^?1), respectively. Levels of other type A and B trichothecenes played a minor role, although the rates of contamination were often high. Neither macrocyclic type D trichothecenes (satratoxin G and H, verrucarin A, roridin A) nor diacetylverrucarol and verrucarol (type A trichothecenes), were detected in any of the samples.     

Validation data for HPLC/FLD determinations of ochratoxin A in red paprika and black pepper adopting a one-step clean-up procedure

Validation data for the determination of ochratoxin A (OTA) in two spice matrices, red paprika and black pepper, were obtained for samples prepared with a simplified single-step clean-up column. Extracts of finely ground samples of red paprika and black pepper were prepared and applied to a Mycosep® 229 Ochra clean-up column. The purified extract was then subjected to HPLC/FLD analysis. The relative standard deviation for repeatability (RSDr) of the method was 11.8% for red paprika and 9.9% for black pepper. The limit of detection (LOD) value (three times the noise) was estimated as corresponding to the response of an extract derived from a blank matrix (previously washed) and spiked at 1.0 µg kg^?1. The limit of quantitation (LOQ) (three times LOD) was 3.0 µg kg^?1. The performance of the one-step column clean-up procedure appears to be a suitable alternative to commonly used clean-up techniques and allows the precise determination of OTA in two complex matrices.     

Survey of furan in foods and coffees from five European Union countries

Canned and jarred baby foods (74), canned and jarred adult foods (63) and 70 coffees sold in Belgium, Italy, Portugal, Spain and The Netherlands were analysed for their furan content using a validated automated headspace GC–MS procedure. Seven balsamic vinegars from Italy and Spain were also analysed. All 74 baby food samples contained detectable furan, with an average level of 37 ng/g. A total of 54 of 63 canned and jarred foods contained detectable furan with an average level of 24 ng/g. Levels of furan in coffee as consumed were very variable and reflected different preparation methods and coffee strengths. Over 50% of Italian samples contained more than 200 ng/g, whereas over 20% of Belgian coffees contained less than 21 ng/g furan. Some brews made from fine grained coffee contained much more furan than did brews made from normal or coarse grained coffee. Although furan was low in most instant coffees, two Italian products “instant espresso” and “instant mocha” contained about 150 ng/g furan. Balsamic vinegars from Spain contained 159–662 ng/g of furan; however, other samples from Spain and Italy contained only 6–25 ng/g.     

Liquid chromatography-tandem mass spectrometry method for the determination of anthelmintics in alfalfa plants

A simple and inexpensive liquid chromatography-tandem mass spectrometric method for the determination of anthelmintics in alfalfa plants (Medicago sativa L.) was developed and validated. Anthelmintics in plant leaves and stems (green chops) were extracted with methanol/acetonitrile (7:3, v/v) followed by a concentration and clean-up step using solid-phase extraction (Strata-X, 500?mg, 6?ml cartridge). After drying with nitrogen gas, the adsorbed analytes were eluted with methanol/acetonitrile (50:50, v/v) mixture followed by 100% acetonitrile. Chromatographic separation was achieved on an Atlantis T-3 (2.1?×?100?mm?×?3?µm) analytical column with a Phenomenex guard cartridge (C8, 4?×?3?mm) attached to a Waters triple quadrupole mass spectrometer operated in positive electrospray ionisation mode with selected reaction monitoring. Samples were analysed using gradient elution at a flow rate of 0.35?ml?min^–1. The mobile phase consisted of a 10?mM ammonium formate solution in (A) water/acetonitrile (90:10, v/v) and (B) methanol/acetonitrile (50:50, v/v). The method was validated for levamisole, fenbendazole, fenbendazole sulphoxide and fenbendazole sulphone at 10, 20 and 40?µg?kg^–1 and for eprinomectin at 20, 40 and 80?µg?kg^–1. Limits of quantification (LOQ) were 10?µg?kg^–1 for all analytes except eprinomectin, which had an LOQ of 20?µg?kg^–1. The overall mean recovery in green plants was between 74.2% and 81.4% with repeatabilities ranging from 2.2% to 19.1% and reproducibilities in the range 3.8–8.7%. The validated method was applied to plant samples in a study on the behaviour of anthelmintic drugs in a soil, plant and water system.