In-house method validation,estimating measurement uncertainty and the occurrence of fumonisin B1 in samples of Brazilian commercial rice

Fumonisin B₁ was investigated in samples of rice intended for human consumption, including polished parboiled rice, whole grain rice and whole grain parboiled rice. Until the present, no studies on the occurrence of fumonisin B₁ have been performed on these types of rice that are commercially available in the south-eastern region of Brazil. A careful intralaboratory validation was carried out to demonstrate the fitness-of-purpose of the applied method for determining fumonisin B₁ in the three studied rice types. The performance criteria – selectivity, reliable limits of detection (50 μg kg⁻¹) and quantification (100 μg kg⁻¹), linearity (range 100–2500 μg kg⁻¹), precision (RSD values ≤ 17.0%) and recovery (71.7–112.0 %) were evaluated, and the expanded measurement uncertainty was estimated by using the data obtained from precision and recovery experiments. Matrix-matched calibration standards were employed to quantify the mycotoxin levels in the rice samples, in which the residual normality, homoscedasticity and independence were confirmed. In addition, the measurement uncertainty values are consistent with the maximum acceptable uncertainty established by European Union regulation for analytical methods for controlling mycotoxins in foodstuffs. Among the thirty-one commercial samples of rice analysed in the present study, five samples presented detectable levels of the mycotoxin, and these levels ranged from 64.8 to 163.0 μg kg⁻¹.     

Occurrence of four mycotoxins in cereal and oil products in Yangtze Delta region of China and their food safety risks

A total of 76 cereal and oil products collected from Yangtze Delta region of China were analyzed for occurrences of aflatoxins (AFs), aflatoxin B₁ (AFB₁), ochratoxin A (OTA), deoxynivalenol (DON) and zearalenone (ZEN). The mycotoxins were determined by the standard detection procedures using immunoaffinity column clean-up coupled with fluorometer (or HPLC-UV). ZEN was the most prevalent toxin, with the incidence of 27.6% (range = 10.0–440.0 μg kg⁻¹), and 9.2% of the evaluated samples were contaminated with a concentration higher than that of the legislation limit of China (60 μg kg⁻¹). AFs and AFB₁ were detected in 14.5% of the samples analyzed, the concentrations ranging 1.1–35.0 μg kg⁻¹ for AFs, and 1.0–32.2 μg kg⁻¹ for AFB₁; 4.0% of the samples had the concentrations of AFs and AFB₁ higher than that of the corresponding legislation limits of China (5.0, 10.0 and 20.0 μg kg⁻¹ for different products). OTA was detected in 14.5% of the cereal and oil products collected; the concentrations ranged 0.51–16.2 μg kg⁻¹. Only 2 samples showed OTA levels higher than that of the legislation limit of China (5.0 μg kg⁻¹). DON was detected in 7.9% of the samples; the concentrations ranged 100–700 μg kg⁻¹, and none of the samples showed DON concentration higher than that of the legislation limit of China (1.0 mg kg⁻¹). A total of 15.8% cereal and oil products were contaminated with at least two mycotoxins (multiple contaminations with different combinations including AFs-ZEN, AFs-OTA-ZEN, OTA-ZEN, ZEN-DON, OTA-ZEN-DON). The dietary exposure assessment results indicated that AFs (AFB₁), OTA, DON and ZEN from cereal-based products represented a series health risk to both adults and children in Yangtze Delta region of China. This is the first report of safety evaluation associated with major mycotoxins for the area.     

Determination of aflatoxins in walnut sujuk and Turkish delight by HPLC-FLD method

This study aims to assess the risk of aflatoxins (AFs) in traditional confectionery products (walnut sujuk and Turkish delight) of Turkey. A high performance liquid chromatography coupled with fluorescence detection (HPLC-FLD) method was used for the determination of AFs. Evaluation of the method showed good selectivity, linearity, recovery and precision. The limit of quantification (LOQ) ranged from 0.106 to 0.374 μg kg⁻¹. The expanded measurement uncertainty was less than 40% for all target analytes. The validated method was successfully applied to the determination of AFs in 112 traditional confectionery products containing nuts (hazelnuts and walnuts). AFs were detected in 43.8% of walnuts and 60.9% of hazelnuts used as ingredients in walnut sujuk and Turkish delight and at levels ranging from 0.58 to 15.2 μg kg⁻¹ and 0.43–63.4 μg kg⁻¹, respectively. This means that AFs levels in walnut sujuk and Turkish delight were up to levels of 6.1 and 9.5 μg kg⁻¹, respectively. Six walnut samples and twenty-one hazelnut samples were above the EU maximum limits (MLs) of 2 and 5 μg kg⁻¹ for aflatoxin B₁ (AFB₁), respectively.     

Survey of aflatoxins and ochratoxin a contamination in food products imported in Italy

In this study the levels of aflatoxins (AF B₁, B₂, G₁ and G₂) and ochratoxin A (OTA) were monitored in several food products imported in Italy with a high contamination risk. A total of 345 samples were collected from the Maritime Authority of Salerno Customs Port during the period from January 2008 to December 2009 and analyzed by immunoaffinity chromatography as clean-up, high performance liquid chromatography with fluorescence detection for quantification and tandem mass spectrometry for confirmation. The analytical methods were validated on different food matrices and meet the performance criteria set by EC Regulation No. 401/2006 for mycotoxin analysis. The results obtained in this survey showed that 7% of the total samples contained detectable levels of AFs and OTA, and 1.2% had AFs concentrations exceeding the maximum limits set by EU regulation. OTA was the most prevalent mycotoxin, with an incidence of 17.6% of samples analyzed for OTA. The highest detected levels were 23.70 μg kg^?1 of OTA in a green coffee sample and 70.69 μg kg^?1 of AFs in an apricot kernels sample. Among the food products analyzed, hazelnuts paste and dried vine fruits were the commodities mainly contaminated with AFs and OTA, respectively.     

Inactivation of aflatoxigenic fungi and the reduction of aflatoxin B1 in vitro and in situ using gamma irradiation

Detailed investigation on the effect of gamma (γ) irradiation on germination, sporulation, and growth of aflatoxigenic moulds (Aspergillus parasiticus 2999, Aspergillus flavus 305, and Aspergillus niger 388), as well as on the reduction of aflatoxin B₁ (AFB₁) level in artificially and naturally contaminated maize/feed samples was performed. The results of in vitro and in situ experiments with aflatoxigenic moulds demonstrated that 5 kGy-γ irradiation manages to prevent sporulation, germination and growth of the tested moulds both when in form of a pure and when in form of a mixed culture. In the feed samples artificially contaminated with AFB₁ (50 μg kg⁻¹) 5 kGy-γ irradiation reduced AFB₁ level by around 60%, while 10 kGy-dose reduce it for around 85%. Similarly, in feed samples spiked with AFB₁ in the concentrations of 100 μg kg⁻¹ 5 kGy-dose reduced the AFB₁ level by approximately 70%, while the dose of 10 kGy reduced it by approximately 90%. The experiments on naturally contaminated maize samples (n = 30) confirmed these observations; following a 5 kGy-irradiation, the overall mean AFB₁ reduction equalled to 69.8%, while the irradiation with a 10 kGy-dose achieved the overall mean toxin reduction of 94.5%. The obtained results indicate that γ irradiation can be used to prevent the growth of aflatoxigenic moulds and to reduce the AFB₁ levels in various goods intended for animal and human consumption, thus minimizing the animal and human exposure to this carcinogenic mycotoxin.     

Co-occurrence of aflatoxins and ochratoxin A in cereal flours commercialised in Turkey

In this study, we aim to determine co-occurrence of aflatoxins (AFs) and ochratoxin A (OTA) in cereal flours commercialised in Corum, Turkey. One hundred cereal flours were checked for target fungal metabolites between the years 2011 and 2013. The samples were analysed by high-performance liquid chromatography with fluorescence detection (HPLC-FLD) after immunoaffinity column (IAC) clean-up procedure. The method was successfully validated in accordance to European Union guidelines acceptance criteria for specificity, linearity, sensitivity, trueness and repeatability. All the results are well below the maximum limits specified in the EU legislation. AFs were detected neither wheat flour nor rice flour samples, while 66.7% of maize flours contained AFs with maximum concentration of 1.12 μg kg⁻¹. OTA was present in 26.7% of wheat flour, 41.7% of maize flour and 18.8% of rice flour samples, with mean levels of 0.247, 0.218 and 0.154 μg kg⁻¹, respectively. The co-occurence of AFs and OTA was found in 9 maize flour samples.     

Occurrence and co-occurrence of Fusarium mycotoxins in wheat grains and wheat flour from Romania

In this study, the presence of fourteen Fusarium mycotoxins, legislated by the European Union – deoxynivalenol, zearalenone, HT-2 and T-2 toxins (EC/1881/2006; 2013/165/EU), or non-legislated (five trichothecens and five “emerging” mycotoxins), was evaluated in 31 whole unprocessed wheat samples and 35 white wheat flour samples from different areas of Romania. For this purpose, a validated multi-mycotoxins liquid chromatography tandem mass spectrometry method was applied. Seventy three percent of the analyzed samples contained at least one mycotoxin. The highest occurrence was for enniatin B, 71% of the analyzed samples being positive (21–407 μg kg⁻¹). Regarding the legislated mycotoxins, deoxynivalenol was detected in 14% (111–1787 μg kg⁻¹) of the samples, while zearalenone was detected in 9% (51–1135 μg kg⁻¹). Only one sample was positive for neosolaniol. Concerning the co-occurrence, 42% of the samples were contaminated with two to five mycotoxins, the most frequent being the binary or tertiary combinations of enniatins. This is the first study applied to Romanian wheat grains and flour samples using a high sensitive multi-mycotoxins method, and which included also “emerging” mycotoxins.     

Aflatoxin and fumonisin contamination of yam flour from markets in Nigeria

The natural occurrence of aflatoxins (AFs) and fumonisins (FBs) in yam flour samples (n = 100) obtained in south-western Nigeria was evaluated. AFs were determined by HPLC with fluorescence detection and FBs by HPLC coupled with mass spectrometry. Aflatoxin B₁ (AFB₁) and aflatoxin G₁ (AFG₁) were found in 57% and 21% of flours from white yam with concentrations ranging from <0.02 (limit of detection, LOD) to 3.2 μg kg⁻¹ (mean = 0.4 μg kg⁻¹) and from <0.05 to 3.5 μg kg⁻¹, respectively. AFB₁ was the only aflatoxin detected in samples from water yam, contaminating 32% of the samples with values ranging from <LOD to 0.6 μg kg⁻¹ (mean = 0.1 μg kg⁻¹). Fumonisin B₁ was found in 32% of the white yam samples (<0.5 (LOD) to 91 μg kg⁻¹; mean = 5 μg kg⁻¹) and in 5% of water yam samples (<LOD to 2 μg kg⁻¹). AFs and FBs were significantly higher (P < 0.05) in white yam flours compared to water yam flours. Preparation of amala from naturally-contaminated yam flour resulted in reduction of AFB₁ and AFG₁ by 44% and 51% respectively. From this study, only 7% of the samples contained AFs above the European standard limits for cereals intended for direct human consumption, while all the FBs-positive samples were well below the limits. The occurrence of ochratoxin A, zearalenone and deoxynivalenol was also evaluated in 20 samples; these mycotoxins were never detected.     

Evaluation of dispersive liquid–liquid microextraction for the determination of patulin in apple juices using micellar electrokinetic capillary chromatography

Patulin (PAT) is a mycotoxin naturally found in fruits, including apples. Its occurrence as a natural contaminant of fruit juices is indicative of fruit quality in production. The European Union has set the maximum content of patulin in 50 μg kg⁻¹ for fruit juices and 10 μg kg⁻¹ for infant fruit juices. In this paper, dispersive liquid–liquid microextraction (DLLME) has been proposed for the extraction and preconcentration of PAT in apple juice, followed by its determination by micellar electrokinetic chromatography (MEKC) with diode-array detection. PAT has been analyzed in the presence of 5-hydroxymethylfurfural (HMF), which is the main interference in this kind of matrix. Variables affecting DLLME efficiency were optimized and the calibration curve was established for PAT in analyte standard solutions, applying the DLLME–MEKC procedure. The limit of detection was 0.6 μg L⁻¹ and recoveries obtained for spiked freshly-made apple juice samples at four different concentration levels (5, 20, 50 and 75 μg L⁻¹), were above 75% with RSD lower than 9%. This method can be classified as a green alternative, being successfully applied to the measurement of 19 apple juice samples obtained from different suppliers and supermarkets. The optimized DLLME–MEKC method is free from matrix effects and avoids the tedious matrix-matched or standard addition calibration method. Almost fifty percent of the samples were contaminated with a PAT content greater than the maximum content established by the European regulation.     

Multiple mycotoxin co-occurrence in maize grown in three agro-ecological zones of Tanzania

In this study, the co-occurrence of multiple mycotoxins in maize kernels collected from 300 households' stores in three agro-ecological zones in Tanzania was evaluated by using ultra high performance liquid chromatography/time-of-flight mass spectrometry (TOFMS) with a QuEChERS-based procedure as sample treatment. This method was validated for the analysis of the main eleven mycotoxins of health concern that can occur in maize: aflatoxin B₁ (AFB₁), aflatoxin B₂ (AFB₂), aflatoxin G₁ (AFG₁), aflatoxin G₂ (AFG₂), ochratoxin A (OTA), deoxynivalenol (DON), fumonisin B₁ (FB₁), fumonisin B₂ (FB₂), HT-2 toxin, T-2 toxin and zearalenone (ZEN). From each zone one major maize producing district for home consumption was chosen and 20 villages for each district were randomly selected for sampling. All mycotoxins of health concern, except for T-2 toxin, were detected in the maize samples. Particularly high levels of AFB₁ (50%; 3–1,081 μg kg⁻¹), FB₁ (73%; 16–18,184 μg kg⁻¹), FB₂ (48%; 178–38,217 μg kg⁻¹) and DON (63%; 68–2,196 μg kg⁻¹) were observed. Some samples exceeded the maximum limits set in Tanzania for aflatoxins or in European regulations for other mycotoxins in unprocessed maize. Eighty seven percent of samples were contaminated with more than one mycotoxin, with 45% of samples co-contaminated by carcinogenic mycotoxins, aflatoxins and fumonisins. Significant differences in contamination pattern were observed among the three agro-ecological zones. The high incidence and at high levels (for some) of these mycotoxins in maize may have serious implications on the health of the consumers since maize constitute the staple food of most Tanzanian population. Effective strategies targeting more than one mycotoxin are encouraged to reduce contamination of maize with mycotoxins.     

A survey of mycotoxins in random street-vended snacks from Lagos,Nigeria, using QuEChERS-HPLC-MS/MS

A survey in African snacks was carried out in order to evaluate the intake of 23 mycotoxins. The African snack samples were purchased from street vendors within Lagos metropolis (Nigeria) and evaluated for the presence of 23 mycotoxins using a modified QuEChERS procedure coupled with liquid chromatography-triple quadrupole linear ion trap mass spectrometer. The snacks included akara, baked coconut, coconut candy, donkwa, groundnut cake (kulikuli), lafun, milk curd (wara), fresh and dried tiger-nuts, and yam flour. Only three mycotoxins were detected in 23.8% of the studied snacks, and at concentrations ranging from 6 to 54 μg kg⁻¹. The concentrations of aflatoxin B₁ (AFB₁) and AFB₂ reached 23 μg kg⁻¹ and 3 μg kg⁻¹, respectively. Moreover a sample of baked coconut contained α-zearalenol (α-ZOL), which was up to 54 μg kg⁻¹ in coconut candy. As considers prevalence, aflatoxins and α-ZOL were not detected in lafun and groundnut-based snacks (donkwa and kulikuli), whereas each of the three mycotoxins contaminated 12.5% (1/8) of the coconut-based samples. This is the first report of α-ZOL in cassava and coconut, and their products. AFB₁ and total aflatoxins (TAFs) concentrations exceeded the maximum allowable limit recommended by National Agency for Food and Drug Administration and Control Nigeria (NAFDAC) in one sample of baked coconut (AFB₁ = 23 μg kg⁻¹ and TAFs = 26 μg kg⁻¹) and donkwa (AFB₁ = 19 μg kg⁻¹ and TAFs = 21 μg kg⁻¹).     

Development and validation of a new qualitative ELISA screening for multiresidue detection of sulfonamides in food and feed

An indirect competitive enzyme-linked immunosorbent assay (ELISA) to screen sulfonamide residues in food (muscle, eggs, milk and honey) and feed has been developed and validated according to Commission Decision 2002/657/EC. The immunoreagents were appropriately produced to detect a wide range of sulfonamide antibiotic congeners, obtaining half-maximum inhibition concentration (IC₅₀) values below 10 μg L⁻¹ for 11 sulfonamides widely used in veterinary practices. Taking into account the complexity of involved matrices, specific sample preparation protocols have been optimised combining high method throughput with low detectable concentrations. Accordingly, depending on the congener, the obtained detection capabilities (CCβs) were lower or equal to 20 μg kg⁻¹ (muscle, eggs and milk), 10 μg kg⁻¹ (honey) and 2 mg kg⁻¹ (feed). Finally the developed qualitative test was applied to real samples collected within the official monitoring programmes: results exceeding the established screening cut-off were re-analysed with a suitable confirmatory method. The presence of one or more sulfonamides was found in all the suspect screening samples thus demonstrating that the proposed ELISA can be successfully applied in class-specific detection of sulfonamides in food and feed.     

Multi-class determination of pesticides and mycotoxins in isoflavones supplements obtained from soy by liquid chromatography coupled to Orbitrap high resolution mass spectrometry

A methodology has been developed to identify and quantify 257 toxic substances (including pesticides and mycotoxins) in diverse isoflavones supplements obtained from soy. Two different extraction procedures were compared, QuEChERS and “dilute and shoot”. The best results were observed when the “dilute and shoot” methodology was applied using acetonitrile acidified with formic acid (1% v/v) as extraction solvent followed by a clean-up step with Florisil cartridges. Validation of the method was carried out evaluating trueness, repeatability and intermediate precision, obtaining recoveries between 70 and 120% with relative standard deviation (RSD) values lower than 20%. Limits of detection and quantification were below 5 and 10 μg kg⁻¹ respectively. The validated methodology was applied to the analysis of real samples, finding pesticides such as flutolanil (12.2 μg kg⁻¹) and etofenprox (48.2 μg kg⁻¹). Regarding mycotoxins, aflatoxin B1 (8.2–17.1 μg kg⁻¹) and aflatoxin G2 (6.4 μg kg⁻¹) were detected.     

Aflatoxins and ochratoxin A in dried eggplant and green bell pepper

In this study, 50 dried eggplant and 50 dried green bell pepper samples were analyzed in terms of their aflatoxin and ochratoxin A (OTA) content. Aflatoxins G₂, G₁, B₂, and B₁, and OTA contents were analyzed using high-performance liquid chromatography with a flame ionization detector (HPLC–FID). Total aflatoxin and, as well as aflatoxin G₂, G₁, B₂, and B₁ content in dried eggplant samples were ranged between 0.82 and 2.58, 0.10–0.23, 0.32–1.35, 0.12–0.67, and 0.17–0.71 μg kg⁻¹, respectively. Total aflatoxin and, as well as aflatoxin G₂, G₁, B₂ and B₁ content in dried green bell pepper samples were 0.81–2.42, 0.11–0.22, 0.32–1.38, 0.13–0.66, and 0.18–0.91 μg kg⁻¹, respectively. OTA content was varied from 8.88 to 21.35 μg kg⁻¹ in eggplant samples, and from 15.38 to 24.70 μg kg⁻¹ in dried green bell pepper samples. Of the dried eggplant samples and dried green bell pepper samples, 36% and 24% of them, respectively, had aflatoxin B₁ values which were below the minimum limit of detection (LOD) of 0.05 μg kg⁻¹. None of the analyzed samples exceeded the legal limit values of 10 μg kg⁻¹ for total aflatoxin content, and 5 μg kg⁻¹ for aflatoxin B₁ content. However, 80% of the dried eggplant samples and 100% of the dried green bell pepper samples exceeded the legal limit value for OTA content (15 μg kg⁻¹). According to the results, it was concluded that dried vegetables should be examined in terms of their aflatoxins. It is essential to analyze OTA content more thoroughly, as it has the potential to pose a risk for public health, as well as for the economy.     

Application of solid phase extraction and two-dimensional gas chromatography coupled with time-of-flight mass spectrometry for fast analysis of polycyclic aromatic hydrocarbons in vegetable oils

A fast and simple solid-phase extraction (SPE) method followed by comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC × GC–TOFMS) has been developed for analysis of 15 + 1 carcinogenic polycyclic aromatic hydrocarbons (PAHs) in vegetable oils. Of three critically assessed sample preparation approaches – (i) gel permeation chromatography (GPC), (ii) GPC followed by silica based SPE, and (iii) SPE employing PAHs-dedicated molecularly imprinted polymers (MIPs), the latter one was selected as the best option. Recoveries of the overall analytical procedure ranged from 70 to 99%, with repeatabilities in the range of 2–11%. Limits of quantitation (LOQs) ranging for individual PAHs from 0.1 to 0.3 μg kg⁻¹, were fairly below the maximum level 2 μg kg⁻¹ established for the PAHs representative, benzo[a]pyrene (BaP), by EU Legislation for this commodity. Within the mini-survey in which the new method was employed for examination of 35 samples of various kinds of vegetable oils collected at the Czech market, the highest PAH4 levels, i.e. the sum of BaP, benz[a]anthracene (BaA), benzo[b]fluoranthene (BbFA) and chrysene (CHR) were found in sea buckthorn (708 μg kg⁻¹) followed by rapeseed oil (99.8 μg kg⁻¹). Altogether 8 samples from 35 examined vegetable oils exceeded the maximum limit 2 μg kg⁻¹ for BaP and 10 samples exceeded 10 μg kg⁻¹ set for PAH4 which is fixed by Commission Regulation (EU) no 835/2011 for oils.     

Deoxynivalenol in the wheat milling process and wheat-based products and daily intake estimates for the Southern Brazilian population

Fusarium head blight of wheat is caused by the Fusarium species that produces mycotoxins, such as deoxynivalenol (DON). The distribution of DON in wheat products can lead to high economic and health impacts. The objective of this study was to evaluate the natural distribution of DON in the wheat milling process and wheat-based products, as well as the daily intake estimates for the Southern Brazilian population. The fractions of wheat grains (milled wheat, finished flour and bran) were produced in a mill. Additionally, wheat-derived products, such as pasta, bread and crackers were analyzed. The bran fraction had the highest mean concentration of DON (2278 μg kg⁻¹), followed by milled wheat and finished flour (1895 μg kg⁻¹ and 1305 μg kg⁻¹). The distribution factor in the finished flour (69%) fraction demonstrates that DON was reduced when compared to milled wheat, by contrast of bran fraction that presents higher DON levels (120%). A percentage of 35% bran, 35% finished flour and 30% milled wheat samples would not be in compliance with future Brazilian regulations for DON levels. From the wheat-based products analyzed, 17% of whole bread and 10% of salted cracker products were contaminated with DON, with a median of 437 μg kg⁻¹ and 624 μg kg⁻¹, respectively. The finished flour was the fraction that most contributes to the daily intake of DON in Southern Brazil, representing 89.6% of the provisional maximum tolerable daily intake.     

A survey on the occurrence of aflatoxin M1 in raw milk produced in Adana province of Turkey

During 2012, a total of 176 samples of raw milk obtained from dairy plants of Adana province of Turkey were analysed for the presence of aflatoxin M₁ (AFM₁). Aflatoxin M₁ analysis was carried out by centrifugation, liquid–liquid extraction, immunoaffinity column clean-up and high performance liquid chromatography with fluorescence detection (HPLC-FD). The limits of detection (LOD) and quantification (LOQ) of the analytical method were 0.021 μg kg⁻¹ and 0.025 μg kg⁻¹. Accuracy of the method obtained from bias ranged from 2.94 to 8.70. Aflatoxin M₁ was detected in 53 out of 176 samples analysed (30.1%). The ranges for positive samples were 0.042–0.552, 0.033–1.01, 0.047–0.150 and 0.025–0.102 μg kg⁻¹ in autumn, winter, spring and summer seasons, respectively. Thirty samples of raw milk (17%) were above the legal limits of Turkey and EU regulations.     

Occurrence of volatile and non-volatile N-nitrosamines in processed meat products and the role of heat treatment

Most of the available data on the occurrence of N-nitrosamines (NA) in processed meat products have been generated in the 1980s and 1990s and especially data on the occurrence of non-volatile NA (NVNA) are scarce. Therefore we have studied the levels of volatile nitrosamines (VNA) and NVNA in processed meat products on the Danish market (N = 70) and for comparison also products on the Belgian market (N = 20). The effect of heat treatment on the NA levels, in selected samples, was also studied, in order to enable an evaluation of how preparation before consumption affects the levels of NA. For the Danish products the mean levels of the VNA were generally low (≤0.8  μg kg⁻¹), whereas the mean levels of the NVNA were considerably higher (≤118 μg kg⁻¹). Slightly higher mean levels were indicated for the Belgian products (i.e. VNA ≤1.5  μg kg⁻¹ and NVNA ≤270 μg kg⁻¹). The sums of VNA were higher than 10 μg kg⁻¹ for one Danish sample and two Belgian samples. Levels of up to 2000 and 4000 μg kg⁻¹ of N-nitroso-thiazolidine-4-carboxylic acid (NTCA) an NVNA occurred in the Danish and the Belgian samples, respectively. The majority of the Danish processed meat products contain NVNA but also VNA occur. The levels of NA are comparable with those reported in previous and recent studies; however the frequency in which they are found may be lower and thereby also the mean contents. The levels of N-nitrosopiperidine (NPIP) increased by frying and baking, whereas varying impacts were observed for N-nitrosoproline (NPRO), N-nitrosodimethylamine (NDMA), N-nitrosopyrrolidine (NPYR), N-nitrosodiethylamine (NDEA) and N-nitrosomethylaniline (NMA) depending on the type of product and/or the heat treatment. The levels of the NVNA, NTCA and N-nitroso-2-methyl-thiazolidine 4-carboxylic acid (NMTCA) decreased after frying and baking.     

Transfer of chloramphenicol from milk to commercial dairy products – Experimental proof

The purpose of the study was to investigate the chloramphenicol (CAP) residue in dairy products after experimental CAP transferring from milk to butter, sour cream, white cheese and whey. In order to determine the CAP residue in dairy products, the new approach for the extraction process was developed. The original, simple and fast analytical method is based on QuEChERS and LC-MS/MS. The homogenized sample was extracted and partitioned after the adding of sodium chloride with acetonitrile. The experiment was conducted to check if CAP is transferred from milk to dairy products, and also to check the extraction of CAP from the different dairy matrices. Average recovery ranged from 97.8 to 102.8% and within-laboratory reproducibility was lower than 8.7%. The suggested method is sensitive, the calculated limit of decision (CCα) was from 0.06 to 0.10 μg kg⁻¹ and detection capability (CCβ) from 0.08 to 0.15 μg kg⁻¹. The results of the experiment (butter 4.86 μg kg⁻¹, sour cream 3.5 μg kg⁻¹, white cheese 2.36 μg kg⁻¹ and whey 0.14 μg kg⁻¹) and validation demonstrated that this method is suitable for determination and confirmation of CAP in a variety of dairy product matrices.     

Sushi commercialized in Brazil: Organic Hg levels and exposure intake evaluation

The presence of organic mercury (methylmercury) in tuna, salmon and kani sushis marketed in restaurants specialising in Japanese foods (Campinas, São Paulo, Brazil), was investigated by atomic absorption spectrometer with thermal decomposition and amalgamation. Total mercury was analyzed directly, whilst organic mercury was quantified after a previous extraction with toluene in an acid solution, assisted by microwaves. Under these analytical conditions there was no interconversion between the inorganic and organic mercury. High sensitivity was observed for organic mercury, with limits of detection and quantification of 2.0 and 6.6 μg kg⁻¹. The organic mercury contents ranged from 12 to 583 μg kg⁻¹, 6.6 to 8.2 μg kg⁻¹ and no detected values, for the tuna, kani and salmon sushi, respectively. The mean proportion of organic Hg/total Hg for tuna sushi was 88%, indicating that the most toxic form of mercury, organic Hg, predominate in this food. The estimated exposure to methylmercury was made by taking into account the Provisional Tolerable Weekly Intake (PTWI 1.6 μg/kg) considering the daily consumption of 150 g and 20 g per adults (60 kg) and children (15 kg), respectively. Our results demonstrated that the consumption of tuna sushi may exceed 100% of PTWI.