Aflatoxin M1 (AFM1) contamination in milk is a potential risk for animal and human health. The occurrence of AFM1 in raw milk from Minas Gerais State, Brazil, in different climate conditions was ...evaluated. A total of 129 milk samples were collected from dairy farms in three distinct periods (dry period, transition period and rainy period), and analyzed by enzyme-linked immunoabsorbent assay (ELISA) as screening test. Samples with AFM1 at concentrations above 0.05 μg/L were analyzed by liquid chromatography with fluorescence detection (HPLC-FD) as confirmatory method. All the analyzed samples showed contamination with AFM1. In the three periods, AFM1 was detected at concentrations below the permitted limit of 0.50 μg/L in milk, according to the Brazilian legislation, and 18 samples (13.95%) showed contamination with AFM1 above the permitted limit of 0.05 μg/L established by Codex Alimentarius and European Commission. Milk contamination with AFM1 was significantly affected by climatic conditions, and the highest values were verified in dry period. The AFM1 contamination was lower than the acceptable daily intake (ADI) estimated for Latin America, indicating that milk from this region is safe for human consumption. Control measures to monitor AFM1 in milk are mandatory in tropical climate countries especially in dry periods.
► The occurrence of AFM1 in raw milk from Minas Gerais State, Brazil, in different climate conditions was evaluated. ► The AFM1 concentrations in milk were below the permitted limits established by national legislation. ► Climate conditions influence the AFM1 contamination in raw milk and the estimate daily intake. ► The contamination levels of AFM1 are higher in dry periods.
A multiresidue method for the quantification of 13 sulfonamides in animal feed is described. It involves the application of a modified QuEChERS procedure followed by HPLC–MS/MS (high performance ...liquid chromatography coupled to tandem mass spectrometry) analysis. The best conditions for the extraction solution and PSA (primary secondary amine) mass were determined. After optimization, the method was validated according to the European Commission Decision 2002/657/EC. The validation levels employed were 25, 50 and 75 μg kg−1. Acceptable values were obtained for the following parameters: linearity (0.9864 < r2 < 0.9993), decision limit (50.4 μg kg−1 < CCα < 55.8 μg kg−1), detection capability (50.7 μg kg−1<CCβ < 55.8 μg kg−1), limit of quantification (0.9 μg kg−1 < LOQ < 7.1 μg kg−1), accuracy (86.0 < recovery rates < 106.8), precision (3.6 < repeatability < 19.5), (5.5 < intermediate precision < 21.6), measurement uncertainty (MU) (4.1 < MU < 32.6) and selectivity. These findings met the Codex requirements, which allow for the routine use of the method by the laboratories linked to the Ministry of Agriculture, Livestock and Food Supply of Brazil. Finally, the method was applied to real samples and only one of them showed positive for sulfamethazine, however, with a concentration below the LOQ of the method.
Although beer is one of the most popular alcoholic beverages in the world, there is no specific legislation regarding contaminants, especially mycotoxins, for this product. The present manuscript ...reports the development and validation of an analytical methodology based on the QuEChERS approach, followed by quantification via UHPLC-MS/MS for the simultaneous determination of seventeen mycotoxins in beer. During the validation, amatrix effect was observed for 82% of the analytes. Linearity and recovery were evaluated using spiked blank samples, and the chosen methodology proved to be efficient for all analytes, with recoveries ranging from 71 to 118%, excepting ergonovine, for which recovery of 57% was achieved. Precision was estimated in terms of repeatability and reproducibility, with variations from 2.6 to 28.2% and 9.7 to 28.7%, respectively. The detection (LOD) and quantification (LOQ) limits, determined from the values of CCα and CCβ, ranged from 0.26 to 117 µgkg
−1
and from 0.30 to 135 µgkg
−1
, respectively. Measurement uncertainties were based on the bottom-up methodology, with uncertainties ranging from 0.03 to 17 µgkg
−1
. Finally, thirty-eight beer samples, collected at the local market, were analysed, and 16 of them showed contamination by deoxynivalenol in concentrations ranging from 159 ± 26 µgkg
−1
to 648 ± 106 µgkg
−1
.
In the present study, the occurrence of aflatoxins (AFs) and ochratoxin A (OTA) was evaluated in 123 samples of cocoa beans produced in five Brazilian states. The presence of these mycotoxins was ...determined by high-performance liquid chromatography with fluorescence detection (HPLC-FLD) after immunoaffinity column clean-up. The mean level of total AFs in cocoa beans samples was 5.7 μg.kg
−1
. Four (3.3%) samples exceeded the maximum limit of 10 μg.kg
−1
established by the Brazilian legislation for total AFs. The mean level of OTA contamination was 1.2 μg.kg
−1
, and none of the samples exceeded the maximum limit established by the Brazilian legislation. The co-occurrence of AFs and OTA was observed in 4.9% of the samples. The results of the present study demonstrated that, in relation to the levels of AFs and OTA established by the Brazilian legislation, most samples of cocoa beans analyzed are safe for consumption. This is the first report on the occurrence and levels of AFs and OTA in cocoa beans from the five main Brazilian states producing cocoa. The data in this study provide important information for farmers, traders, industry, consumers and law enforcement agencies.
The aim of this study was to investigate the presence of arsenic, lead, and cadmium residues in samples of liver, kidney, and muscle of cattle during the years of 2002 to 2008. A total of 1017 ...samples from 20 Brazilian States were used. The samples were analyzed at the National Agricultural Laboratory using the atomic absorption spectrometry technique. Arsenic residues were detected in 15.7% of liver samples and 28.7% of kidney samples although no results have exceeded the MRL. With regard to lead, 16 samples of liver and 74 samples of kidney were contaminated (5.2 and 10.9%, respectively). Among these samples, only one liver and two of kidney samples had lead levels above the MRL. Cadmium was found with levels below the MRL in 12.5% of the liver samples, and only 3 samples (1%) were quantified above the MRL. Among the kidney samples, 420 (60.8% of the total tested) had cadmium residues, and five of them exceeded the limits established by legislation. It is concluded that the Brazilian meat meets the legislation requirements without putting consumer's healthy at risk since as it satisfies the national and international food-safety conditions.
A new method for the quantification of four aflatoxins (AFB1, AFB2, AFG1, and AFG2) in baby food samples is described herein. In this method, the extraction/cleanup step was performed by using ...multi-walled carbon nanotubes as a sorbent material in a dispersive solid phase procedure. In sequence, these mycotoxins were quantified via liquid chromatographic coupled with tandem mass spectrometry. The method was fully validated according to the EC/657/2002 and SANCO/12571/2013 directives. Adequate values were obtained for all figures of merit, mainly veracity (recoveries: 75.8 to 120.6%) and quantification limits (LOQs: 60.0 to 560.0 ng kg
-1
), with no noticeable matrix effects. The method was tested in real samples (
n
= 4) and aflatoxin B1 (AFB1) was detected in just one of them. Finally, this analytical procedure has an evident potential to be applied to analyze aflatoxins (and other mycotoxins) in distinct types of complex samples.
In this study, 135 samples of cocoa beans collected in the Amazon and Atlantic Forest regions of Brazil were analysed to evaluate the possible co-occurrence of 34 mycotoxins. The results indicate ...that 42% of the cocoa samples exhibited quantifiable levels for 11 mycotoxins: aflatoxins (AFs) B
1
, B
2
and G
1
; ochratoxin A; citrinin; cyclopiazonic acid; tenuazonic acid; paxilline; sterigmatocystin; zearalenone and fumonisin B
2
. Of the samples, 18% exhibited the co-occurrence of up to six mycotoxins. No toxins belonging to the groups of trichothecenes or ergot alkaloids were detected. Contingency analysis of the incidence of mycotoxins did not show significant differences between the two regions evaluated. Seven samples were contaminated with AFs, while only one contained ochratoxin A above 10 μg kg
−1
. The accuracy of the method was evaluated by proficiency testing for ochratoxin A, where satisfactory Z-scores were obtained.
•A methodology to determine pesticides and mycotoxins in rice was developed.•The method makes use of the dilute and shoot procedure and UHPLC-MS/MS.•The method was validated according to the ...EC/657/2002 normative.•The method was applied in the analysis of rice commercialized in Brazil.•These real rice samples shown to possess quite low levels of these analytes.
In the present manuscript an analytical methodology for the simultaneous determination of ten mycotoxins and six pesticides in rice was developed. This methodology comprises the application of the dilute and shoot protocol followed by quantification via UHPLC-MS/MS. The methodology was validated and all figures of merit shown to be within the limits established by regulation. Hence, the recoveries for mycotoxins and pesticides were within the specified ranges. Precision was assessed by repeatability and intra-laboratory reproducibility with standard deviations smaller than or equal to 20%. The limits of detection, quantification and decision as well as the detection capacity were determined by the analytical curves whereas the measurement uncertainty was established by applying the bottom-up approach. Finally, the current methodology was applied to samples of rice (n = 42) commercialized in Brazil and positive results were found in only two for deoxynivalenol and zearalenone.
This work proposes an extraction method based on the “dilute and shoot” approach and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) for the simultaneous determination of 42 mycotoxins (34 ...quantified and 8 qualitatively studied) in dried cocoa bean samples. The purpose of the developed methodology was the reduction of co-extractives from the matrix and an efficient extraction without a cleanup step, and subsequent analysis by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). In order to obtain the best extraction conditions, gravimetric tests were performed and parameters that influenced the extraction efficiency were evaluated, such as the proportion of extraction phases, amount of salt, acidification, and extraction time. The performance of the developed method was evaluated to ensure its reliability. Considering the recovery range of 70–120% as an accuracy parameter, four of the mycotoxins under study (acetyl T-2, tenuazonic acid, wortmannin, and zearalenone) showed undesirable values at one of the levels evaluated. The repeatability of the method was assessed for 34 mycotoxins by the relative standard deviation (RSD%) of the responses, and all presented satisfactory values. The quantification limits ranged from 1.0 to 33.0 μg kg
−1
. Modification of the extraction methods made it possible to simultaneously analyze multiple mycotoxins, eliminating the need for the cleanup step, which led to analyte losses. The proposed methodology has a low cost, which makes it advantageous in routine analysis. It also has the potential for scope extension to cocoa-based foods, which are naturally exposed to a greater variety of mycotoxins.
Graphical abstract
A collaborative study was conducted to evaluate a method using immunoaffinity column cleanup with liquid chromatography (LC) for the determination of ochratoxin A (OTA) in green coffee at levels that ...could be included in possible future regulations of the European Union. The test portion was extracted with methanol-3% aqueous sodium hydrogen carbonate solution (50 + 50, v/v). The extract was filtered, and the filtrate was diluted with phosphate-buffered saline and applied to an immunoaffinity column containing antibodies specific for OTA. After washing, the toxin was eluted from the column with methanol and quantified by LC with fluorescence detection. Pairs of 4 homogeneous noncontaminated and naturally contaminated materials (mean levels of < 0.12, 2.44, 5.15, and 13.46 ng/g) and blank samples (< 0.12 ng/g) for spiking were sent to 20 participant laboratories from 8 countries. The materials were analyzed according to the method description and all difficulties encountered in the analysis were reported. Statistical analysis was carried out according to the Harmonized Protocol of the International Union of Pure and Applied Chemistry. The relative standard deviation for repeatability (RSDr) ranged from 7.42 to 20.94%, and the relative standard deviation for reproducibility (RSDR) ranged from 16.34 to 29.17%. The method showed acceptable within-laboratory and between-laboratories precision for green coffee materials, as evidenced by HorRat values of < or = 0.85, at the studied range, for spiked and naturally contaminated materials. The mean recovery was 92.8% for green coffee material spiked with OTA at a level of 4.82 ng/g.
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