Occurrence of aflatoxin M1 in pasteurised,UHT milk and milk powder from goat origin

In the present study, 36 samples of pasteurised, ultra-high-temperature (UHT) treated and goat milk powder traded in the city of Campinas, Brazil, were analysed for aflatoxin M₁ (AFM₁), from October to December 2004 and March to May 2005. Results showed 25 (69.4%) positive samples for AFM₁ at levels of 0.011–0.161 μg L⁻¹ of milk, which were below the tolerance limit of 0.500 μg L⁻¹ as adopted for AFM₁ in milk by Brazilian regulations. Mean levels of AFM₁ in pasteurised, UHT and goat milk powder were 0.072 ± 0.048, 0.058 ± 0.044 and 0.056 ± 0.031 μg L⁻¹, respectively. It is concluded that the incidence of AFM₁ in goat milk traded in Campinas is high, but at levels that probably leads to a non-significant human exposure to AFM₁ by consumption of goat milks.     

Incidence and level of patulin contamination in pure and mixed apple juices marketed in Italy

A survey on the occurrence of patulin was conducted during 2005 on commercial pure apple juices (53 samples) and mixed apple juices (82 samples) marketed in Italy. The current study was undertaken to investigate the possible influence of the agro-food production process employed (conventional or organic), of the fruit percentage in the commercial product (higher or lower than 50%) and of the type of apple juice (clear or cloudy) on the occurrence and level of patulin contamination. Patulin could be quantified in 34.8% of the samples ranging from 1.58 to 55.41 μg kg⁻¹. With the exception of one sample, the level of patulin was lower than 50 μg kg⁻¹, the maximum permitted threshold in fruit juices according to the European legislation. Mean levels of patulin were significantly lower in mixed apple juices (4.54 μg kg⁻¹) than in pure apple juices (9.32 μg kg⁻¹). Levels of patulin contamination were comparable in clear and cloudy juices. A similar incidence of positive samples was found in conventional and organic apple based juices, and the magnitude between the mean contamination levels, although higher in organic (10.92 μg kg⁻¹) than in conventional juices (4.77 μg kg⁻¹), was not statistically significant (p = 0.771; Mann–Whitney test). The magnitude between the means of patulin contamination in juices containing more than 50% fruit (11.26 μg kg⁻¹) and in juices with 50% or less fruit (3.35 μg kg⁻¹) was statistically significant (p = 0.016; Mann–Whitney test).     

Regional monitoring plan regarding the presence of aflatoxin M1 in pasteurized and UHT milk in Italy

The aim of the study involved evaluation of the presence of aflatoxin M₁ in milk for sale in a specific North West Italian region, Piedmont. The study, conducted from November 2003 to July 2005, was linked to the specific emergency situation which arose due to the climatic conditions during the summer of 2003 which encouraged the development of aflatoxin B₁ in items used for animal feed. This in turn led to the transfer of the metabolite, aflatoxin M₁, into the milk. In total some 316 milk samples were collected during the commercial phase by the official control bodies and analysed. The analysis involved the use of high pressure liquid chromatography (HPLC) combined with fluorimetric measurement, and purification of the extracts using immunoaffinity columns. The results indicated only 2 non conforming samples (0.6%), with limits higher than those set out in the regulations (0.05 μg L⁻¹). In addition, the analyses revealed, in 5 samples (1.6%), threshold values of 0.05 μg L⁻¹. From the data obtained it can be seen that the “aflatoxins” problem only marginally affected Piedmont Region though the trend for average monthly values suggests a return to the use of contaminated animal feed as soon as official controls are less intensive.     

Aflatoxins in rice – A limited survey of products marketed in Austria

Eighty-one rice samples were purchased from different markets in Vienna and were analysed for their aflatoxin content. The samples were extracted using methanol in water (80/20 v/v) followed by immunoaffinity clean up. The determination was carried out by HPLC–FLD coupled to a Kobracell. Different samples including basmati rice, whole grain rice, long grain rice, short grain rice as well as puffed rice were investigated. Moreover, conventionally and organically produced rice were compared. The results revealed that 24 out of 81 samples contained detectable amounts of aflatoxins. Aflatoxin B₁ could be quantified in 15 samples and aflatoxin B₂ in one sample. The contamination range was noted to be between 0.45 μg kg⁻¹ and 9.86 μg kg⁻¹ for aflatoxin B₁ and 1.5 μg kg⁻¹ for aflatoxin B₂. Aflatoxins G₁ and G₂ were not detected in any sample. Three samples exceeded the maximum levels set in the European Union; having AFB₁ concentrations of 2.16, 2.85 and 9.86 μg kg⁻¹. In the three organic produced rice samples only traces of aflatoxins were found.     

Occurrence of ochratoxin A before bottling in DOC and DOCG wines produced in Piedmont (Northern Italy)

Italy is one of the countries where ochratoxin A (OTA) contamination in wine poses more risks. Previous surveys on the occurrence of OTA have poorly considered north Italian wines. In this study, 1206 red and white DOC and DOCG wines produced in Piedmont (Northern Italy) from 2000 to 2007 have been analyzed for OTA level (0.116 μg l⁻¹) and incidence (68.0%). The monitoring – the widest per number of Italian wine samples considered – analyzed the OTA contamination of wines in tanks just before bottling. OTA level and incidence were significantly higher in red (0.121 μg l⁻¹, 69.4%) than in white (0.086 μg l⁻¹, 61.3%) wines. Among the white wines, the incidence was significantly lower in the Moscato wines (7.3%), due to the different wine processing. The differences in the mean OTA level in the three main grapevine varieties of red wines could be related to the harvest period. Among the Nebbiolo appellations, a reduction of the OTA level was noticed with increasing the wood aging period. A significant effect of the vintage year was also registered.     

Aflatoxin M1 in raw,pasteurized and powdered milk available in the Syrian market

The incidence of contamination of aflatoxin M1 (AFM1) in milk samples collected from the Syrian market was investigated by using the competitive enzyme linked immunosorbent assay (ELISA) technique. A total of 126 samples composed of raw cow milk (74 samples), raw sheep milk (23), raw goat milk (11), pasteurized cow milk (10) and powdered milk (8) showed that 80% of tested samples were contaminated with various levels of AFM1 ranging from >20 to 765 ng/l. Percentages of AFM1-contaminated samples exceeding the American, Syrian and European tolerance limits were 22%, 38% and 52%, respectively.The range of contamination was relatively higher in pasteurized milk than in raw cow and sheep milk. 80% of AFM1-contaminated pasteurized cow milk samples exceeded the European tolerance limit with a range of contamination between 89 and 765 ng/l. Percentages of contaminated raw cow, sheep and goat milk exceeding the European tolerance limit were 59%, 24% and 14%, respectively.Milk powder was almost free of AFM1 contamination with only one sample containing a concentration lower than the European tolerance limit (12 ng/l).Extrapolation of aflatoxin B1 (AFB1) from AFM1 levels of contamination in milk samples indicates that contamination in dairy cattle feeds may range from 0.5 to 47.8 μg/kg.     

Occurrence of aflatoxin M1 in raw milk in South Korea using an immunoaffinity column and liquid chromatography

The level of aflatoxin M₁ (AFM₁) contamination in raw milk produced in South Korea was investigated using immunoaffinity column chromatography and high performance liquid chromatography with fluorescence detector. A total of 100 raw milk samples were collected from 100 cattle ranches located in three different provinces of South Korea. Forty eight out of 100 raw milk samples contained AFM₁ at low level (0.002–0.08 μg/L) with mean value of 0.026 μg/L. Among the AFM₁ contaminated samples, 29 raw milk samples contained only traceable amount of AFM₁ below the limit of LOQ, 0.02 μg/L. None of samples exceeded the maximum level (0.5 μg/L) of Korean regulation for AFM₁ in milk. The limit of detection was 0.002 μg/L. The result of recovery test with 0.5 μg/L AFM₁ in raw milk sample was 96.3% (SD 3.6, n = 5). This is the first pioneering study to investigate the level of AFM₁ in raw milk used in dairy industries in South Korea.     

Survey of aflatoxin B1 in helva,a traditional Turkish food,by TLC

A total of 102 helva samples consisting of 34 plain helva, 34 helva containing cacao, and 34 helva containing pistachio nuts purchased from helva-factories and supermarkets in Adana of Turkey were analysed for aflatoxin B₁ (AFB₁) by thin-layer chromatography. The detection limit of AFB₁ was 1 μg kg⁻¹. Recovery experiments were carried out with spiked samples in the range 2–10 μg kg⁻¹ of AFB₁. No AFB₁ was found in any plain helva and helva containing cacao samples. On the other hand, of 34 helva containing pistachio nuts AFB₁ was determined in eight samples. AFB₁ was found in excess of Turkish legal limit of 5 μg kg⁻¹ in 4 of 102 helva samples. This paper reports the data of the first survey for the presence of AFB₁ in helva in Turkey.     

Fumonisins in brewers grain (barley) used as dairy cattle feed in the State of Bahia,Brazil

Fumonisins are mycotoxins produced by the genus Fusarium that may induce toxic effects in several animal species and may be found in several kinds of foods and feed. In the State of Bahia, Brazil, brewers grain, which are a brewery by-product, have been largely used in the feeding of animals, specially dairy cattle, due to their nutritional value and low cost of transportation. The aim of this study was to establish the presence of fumonisins in brewers grain used as dairy cattle feed in the State of Bahia. Twenty samples of brewers grain were collected every three months during a whole year, for a total of 80 samples, in five properties located in the “reconcavo baiano”. These samples were analyzed for the presence of fumonisins using high efficiency liquid chromatography (HPLC). Results showed contamination of 58 (72.5%) samples, with contamination mean level equal to 226.5 μg/kg, with 50.30 and 908.47 μg/kg as the minimum and maximum levels, respectively. This is the first report of the occurrence of this mycotoxin in the State of Bahia.     

Aflatoxin M1 contamination in dairy products marketed in Iran during winter and summer

In the present study, 298 dairy product samples consisting of pasteurized milk (91 samples), yoghurt (68 samples), white cheese (72 samples), butter (31 samples) and ice cream (36 samples) collected from popular markets in four large Iranian cities were examined for aflatoxin M₁ (AFM₁) by thin layer chromatography (TLC) technique. The toxin was detected in 66 (72.5%) pasteurized milk samples (mean: 0.052 μg/l; range: 0.013–0.250 μg/l), 45 (66.1%) yoghurt samples (mean: 0.032 μg/kg; range: 0.015–0.119 μg/kg), 59 (81.9%) white cheese samples (mean: 0.297 μg/kg; range: 0.030–1.200 μg/kg), 8 (25.8%) butter samples (mean: 0.005 μg/kg; range: 0.013–0.026 μg/kg) and 25 (69.4%) ice cream samples (mean: 0.041 μg/kg; range: 0.015–0.132 μg/kg). The concentration of AFM₁ in 36.2%, 20.6%, 30.5%, 9.6% and 27.7% of pasteurized milk, yoghurt, white cheese, butter and ice cream samples, respectively, were higher than Iranian national standard limits. Levels of AFM₁ in samples of pasteurized milk, yoghurt, butter and ice cream collected in winter were significantly higher (P < 0.05) than those collected in summer. In the case of white cheese, level of AFM₁ was higher in winter than in summer, but the difference was not statistically significant (P > 0.05). The results indicated that the contamination of the dairy products in such a level could be a serious public health problem at the moment.     

Microbiological quality of legume-based traditional fermented foods marketed in West Bengal,India

A total of 105 samples of six different types of legume-based popular fermented foods, namely amriti, dhokla, dosa, idli, papad and wadi, purchased from retail outlets in West Bengal, was analysed to determine their microbiological safety status. While dhokla and idli were of high-moisture foods (62 g (100 g)⁻¹), others had a lower moisture level (14–27 g (100 g)⁻¹). Papad was alkaline (pH 8.7), whereas all the other foods were acidic (pH 4.4–5.8). Every sample was found contaminated with total aerobic mesophilic bacteria (detection limit, 10 cfu g⁻¹); 38% (40/105) of the samples contained more than 10⁶ cfu g⁻¹. Aerobic mesophilic bacterial spores were found in 88% (92/105) of the samples (detection limit, 100 cfu g⁻¹), whereas their anaerobic counterparts were present in 39% (41/105) of the samples (detection limit, 10 cfu g⁻¹). Although all the samples, excepting one, were free from Staphylococcus aureus (detection limit, 100 cfu g⁻¹), 20% (21/105) of the samples were found contaminated with Bacillus cereus (detection limit, 100 cfu g⁻¹). Enterobacteriaceae were found in 46% (48/105) of the samples (detection limit, 10 cfu g⁻¹). Of the Enterobacteriaceae isolates, 92% were coliforms and 57% were faecal coliforms. Escherichia coli (detection limit, 10 cfu g⁻¹) was found in only one sample each of wadi and idli, at a load of 10³–10⁴ g⁻¹. Salmonella (detection limit, 1 cell (25 g)⁻¹) occurred in 12 samples of wadi, idli and papad, however was absent in the other three products. Clostridium perfringens (detection limit, 10 cfu g⁻¹) and Shigella (detection limit, 1 cell (25 g)⁻¹) could not be detected. The results obtained in the present study indicated that these foods were manufactured using poor-quality starting materials, processed under unhygienic conditions, or/and temperature-abused during transportation and storage. Based on these results, a guideline is recommended for obtaining safe products.     

Optimization of the liquid–liquid extraction method and low temperature purification (LLE–LTP) for pesticide residue analysis in honey samples by gas chromatography

This work optimized a simple and practical method for identification and quantification of the pesticides chlorpyrifos, λ-cyhalothrin, cypermethrin and deltamethrin in honey samples. The method was based on liquid–liquid extraction and low temperature purification using acetonitrile: ethyl acetate (6.5 mL:1.5 mL) as the solvent for extraction. A final clean up step with 2 g florisil was performed before analysis by gas chromatography using electron-capture-detector. The technique was proven satisfactory with efficiency exceeding 85% and linear chromatographic response for the tested pesticides, ranging from 0.033 to 1.7 μg g⁻¹ with correlation coefficients above 0.99. Detection and quantification limits were lower than 0.016 and 0.032 μg g⁻¹, respectively. The proposed method was applied to 11 honey samples. Chlorpyrifos and λ-cyhalothrin residues were found in two samples at concentrations below maximum residue limit (MRL) established for food products. The presence of these compounds was confirmed by mass spectrometry in SIM mode (GC–MS-SIM).     

Dissipation of propisochlor and residue analysis in rice,soil and water under field conditions

The analytical method for the residues of a new herbicide propisochlor and its dissipation and residual amounts in soil, water and rice plants in field conditions (rice cropping system) were studied. The chloroacetanilide herbicide, propisochlor (72% w/w EC) was applied at two dosages, 108 g a.i. ha⁻¹ (recommended) and 162 g a.i. ha⁻¹ (1.5 times of the recommended dosage) seven days after transplanting rice seedlings in the experimental fields in both Beijing and Fujian provinces (experimental localities). Soil, water and rice plant samples were collected at intervals and analyzed for propisochlor residues. The detection limit (LOD) of propisochlor is 0.2 μg kg⁻¹ and the limit of quantification (LOQ) was established as 1 μg kg⁻¹. At three different spiking levels, mean recoveries and relative standard deviation (RSD) from fortified samples in three replicated experiments for each matrix were in the range 81–109% and 1.3–13.1%, respectively. The results showed that the half-lives of propisochlor in water, soil and rice plant from Beijing were 0.56, 5.25 and 1.46 days respectively, and the half-lives of propisochlor in water, soil and rice plant from Fujian were 0.62, 5.12 and 0.81 days. At harvest, soil, straw, rice hull and husked rice samples were found to contain propisochlor well below the limit of detection (LOD) following the recommended dosage and 1.5 times dosage.     

Levels of polychlorinated dibenzo-p-dioxins,dibenzo-p-furans and polychlorinated biphenyls in farmed sea bass (Dicentrarchus labrax) and sea bream (Sparus aurata) from Turkey

Farmed European sea bass and Gilthead sea bream were obtained from four different fish farms in Turkey during 2008–2009, for determination of 17 2,3,7,8-Cl-substituted PCDDs and PCDFs, and coplanar and indicator PCBs.Concentrations of ∑PCDD/Fs and DL-PCBs, as TEQ, in fish samples, ranged from 0.14 to 0.70 pg TEQ₍₁₉₉₈₎ g⁻¹ wet weight and from 0.46 to 4.51 pg TEQ₍₁₉₉₈₎ g⁻¹ wet weight, respectively. The concentrations of total indicator PCBs in fish samples ranged from 3.1 ng g⁻¹ to 22.1 ng g⁻¹ wet weight. Concentrations of PCDD/Fs and DL-PCBs were below the EU regulation (EC No. 1881/2006) limits.     

Immunoaffinity pre-concentration combined with on-column visual detection as a tool for rapid aflatoxin M1 screening in milk

A non-instrumental rapid test was developed for the screening of aflatoxin M1 (AfM1) in milk at the 40 ng/L level. The method combines on one immunoaffinity gel layer, AfM1 pre-concentration and direct competitive immunoassay detection with visual evaluation. Aflatoxin B1-horse radish peroxidase (AfB1-HRP) and Sepharose 4B-immobilized anti-aflatoxin B1 monoclonal antibody with a 79% cross-reaction for AfM1 were used. The assay was performed in a standard column for solid phase extraction using a milk sample volume of 10 mL. Raw milk, pasteurized milk, milk powder, kefir and yogurt were analyzed with the developed test. It was shown that pasteurized milk could be analyzed without any sample preparation. The other types of milk were analyzed after centrifugation. For the assay procedure an aliquot of milk was flowed through the immunoaffinity gel layer in the tube by pushing the plunger of a syringe. Further, AfB1-HRP was applied and bound to free antibody binding sites. After addition of the chromogenic substrate the results were visually evaluated. Blue colour developed in case of negative milk samples while no colour appeared for positive samples. This method showed a false negative rate of only 2% and a high throughput (20–35 min for six samples).     

A HPLC with fluorescence detection method for the determination of tetracyclines residues and evaluation of their stability in honey

A high-performance liquid chromatography with fluorescence detection method for the simultaneous determination of oxytetracycline (OTC), tetracycline (TC) and chlortetracycline (CTC) residues in honey was developed and validated. Sample preparation was done in a single solid phase extraction step. The chromatographic separation was performed on a C₈ column. Matrix matched calibration curves showed linearity higher than 0.99. The accuracy values lay between 86% and 111% and the precision was lower than 11%. Limits of detection and quantitation were 8 μg kg⁻¹ and 25 μg kg⁻¹, respectively. The method was employed to evaluate the stability of the tetracyclines in honey during 60 days of storage. The residue levels of OTC, TC and CTC were reduced 97%, 76% and 71%, respectively. Honey samples (n = 22) collected from the retail market were analyzed. No tetracyclines residues were detected.     

Effect of combined physico-chemical treatments based on enterocin AS-48 on the control of Listeria monocytogenes and Staphylococcus aureus in a model cooked ham

Enterocin AS-48 was tested alone or in combination with chemical preservatives and/or heat against Listeria monocytogenes and Staphylococcus aureus in a cooked ham model system. AS-48 (20, 40 and 60 μg g⁻¹) alone was active against L. monocytogenes at 5 and 15 °C, but it was not sufficient to avoid regrowth of Listeria during the 60 days storage. Combination of AS-48 (40 μg g⁻¹) with nitrite/nitrate, pentasodium tripolyphosphate, sodium benzoate or potassium sorbate improved the anti-listeria effect during storage at 5 °C. The most effective combination was AS-48-nitrite/nitrate (0.007%) that reduced listeria below detection level from the beginning to end of storage. Although much more resistant, S. aureus was also inhibited by AS-48 alone at 5 °C, and especially in combinations with nitrite/nitrate, pentasodium tripolyphosphate, sodium lactate and sodium acetate. Best results against both pathogens were obtained when sodium pyrophosphate was applied in combination with 60 μg g⁻¹ AS-48. Sub-lethal heat (60 °C, 2 min) clearly increased AS-48 activity against both Listeria and Staphylococcus.     

Mycotoxins in food from Jordan: Preliminary survey

This study was undertaken to determine the presence of mycotoxins in foods from Jordan. For this purpose, a total of 108 samples of different groups of foods widely consumed by the Jordanian population were collected during 2008–2009 years. Samples were analyzed for contamination with aflatoxins, ochratoxin A, deoxynivalenol, fumonisins, zearalenone and T-2 toxin by direct competitive enzyme-linked immunosorbent assay (ELISA). The predominant mycotoxin was ochratoxin A with a mean level of 4.17 μg kg⁻¹ in 25% of analyzed samples. Furthermore, aflatoxins, deoxynivalenol and fumonisins were detected with a contamination frequency of 3%, 4% and 2%, respectively. The present report is the first one ever carried out on the occurrence of mycotoxins in food consumed by the Jordanian population.     

A versatile splitless injection GC-FID method for the determination of mineral oil paraffins in vegetable oils and dried fruit

A splitless injection GC-FID method for determining mineral paraffins in food was set up. The method has been developed on vegetable oils and subsequently adjusted and applied to dried fruits, a food matrix not yet investigated from this point of view. The method avoids the saponification step foreseeing only a clean-up on silica gel SPE, and allows the quantification of mineral paraffins with a limit of quantification (LOQ) of 15 mg kg⁻¹ and a detection limit (LOD) of 5 mg kg⁻¹ in the oils. LOQ and LOD for the analysis of dried fruit samples are respectively 1.0 and 0.3 mg kg⁻¹.Eighteen samples of dried fruit were analysed (apricots, plums, raisins, coconut, dates, mango, pineapple). Two samples of apricots showed high values of contamination, 23.0 and 28.2 mg kg⁻¹ of mineral paraffins, while all the other samples contained less than 6.4 mg kg⁻¹ of mineral paraffins and in four samples mineral paraffins were undetectable.     

Antimicrobial effect of acidified sodium chlorite,sodium chlorite,sodium hypochlorite,and citric acid on Escherichia coli O157:H7 and natural microflora of fresh-cut cilantro

Fresh-cut cilantro is particularly susceptible to microbial growth and, therefore, use of an effective sanitizer on this product is of great importance. The objective of this study was to evaluate the efficacy of different sanitizing treatments on reducing Escherichia coli O157:H7 populations, aerobic mesophilic bacterial, yeast and mould counts on fresh-cut cilantro. Cut cilantro was treated with sodium hypochlorite (SH) at 0.2 g L^?1 free chlorine and acidified sodium chlorite (ASC) at 0.1, 0.25, 0.5 and 1 g L^?1, along with the components of ASC, i.e., citric acid (CA) at 6 g L^?1 and sodium chlorite (SC) at 1 g L^?1. In the present study, it was found that SH inactivated, at maximum, 1–1.3 log cfu g^?1 of background or pathogenic microflora present on cut cilantro. However, reductions of more than 3 log cfu g^?1 were observed after washing with 1 g L^?1 of ASC. Moreover, when lower concentrations of ASC were used (0.25 and 0.5 g L^?1), microbial populations were reduced by about 2 log cfu g^?1. SC was as effective as ASC at 1 g L^?1 in reducing aerobic mesophilic bacteria and E. coli O157:H7 populations, although it was not as effective as ASC in reducing yeast and mould populations.