Incidence of patulin in apple juices marketed in Turkey.

The purpose of this study was to investigate the patulin contamination of apple juices consumed by the Turkish population. Patulin was detected using high-performance liquid chromatography (HPLC) with a UV detector at 280 nm, and the identification of patulin was further confirmed by thin-layer chromatography (TLC). Using HPLC, the recoveries were 79.9 +/- 6.7% and 83.7 +/- 4.6%, and the coefficients of variation were 8.4 and 5.5% for apple juices spiked with the known amounts of patulin (60 and 120 microg/liter. respectively). The minimum patulin level detected was 5 ng in a standard solution and 5 microg/liter in apple juices. The TLC method was used only to confirm patulin levels higher than 20 microg/liter (100 ng/spot) in apple juices. The total number of samples was 45. Patulin was present in detectable levels in 60% of apple juices at concentrations ranging from 19.1 to 732.8 microg/liter. Forty-four percent of the apple juice samples had patulin contamination levels higher than 50 microg/ liter, which is the allowable upper limit in Turkey.     

Occurrence of patulin in organic, conventional, and handcrafted apple juices marketed in Belgium

The aim of this research was to compare the occurrence of patulin in a large group of organic, conventional, and handcrafted apple juices marketed in Belgium. An analytical procedure based on high-performance liquid chromatography with UV detection was validated and used to analyze 177 apple juice samples: 65 organic, 90 conventional, and 22 handcrafted. Patulin was detected in 22 samples (12%), and quantification was possible in 10 (6%) of these samples. The patulin content was higher than the European legal limit of 50 microg/liter in two samples of organic apple juice. Although, the incidence of patulin in organic (12%), conventional (13%), and handcrafted (10%) apple juices was not significantly different (P = 0.863), the mean concentration of patulin in contaminated samples was significantly higher in organic (43.1 microg/liter) than in conventional (10.2 microg/liter) (P = 0.02) and handcrafted (10.5 microg/liter) (P = 0.037) apple juice. The highest patulin concentrations were found in the most expensive apple juices because of the higher price of organic apple juice. This relation was not observed when only conventional apple juices were analyzed.     

Occurrence of patulin and its dietary intake through apple juice consumption by the Spanish population

A survey was conducted to determine levels and dietary intake of Patulin (PAT) from apple juices consumed in Spain. One hundred samples of apple juice were bought from distinct supermarkets. PAT was extracted by a liquid–liquid extraction technique and analysed with a micellar electrokinetic chromatography (MEKC) method. 66% of the samples contained PAT over the limit of detection of the method (0.7 μg L⁻¹). The PAT apple juice mean and median levels obtained were 19.4 and 4.8 μg L⁻¹, respectively, in a range between 0.7 and 118.7 μg L⁻¹. In 11% of the samples, PAT contamination exceeded the maximum permitted level of 50 μg L⁻¹ established by the EU regulation. In Spain, no significant variations were observed with respect to data published 15 years ago.     

Incidence of patulin in fruits and fruit juices marketed in Campinas, Brazil

One hundred and eleven samples of processed fruit juices (apple, grape, pineapple, papaya, guava, banana and mango) and 38 samples of sound fruits (apple, papaya, mango, pear and peach) produced and marketed in Brazil, were analysed for patulin by HPLC. Only one out of 30 samples of apple juice was found positive at 17 mug/l. Patulin was not detected in the other foodstuffs. It was found in 14 samples of spoiled fruit samples of apple (150-267 mug/kg), pear (134-245 mug/ kg) and peach (92-174 mug/kg). Confirmation of the identity of patulin was based on the UV spectrum obtained by the HPLC diode array detector, compared with thatof standard patulin, TLC developed by several solvent systems and sprayed with 3-methyl-2-benzothiazolinone hydrazone , and by acetylation with acetic anhydride.     

Occurrence of patulin in conventional and organic fruit products in Italy and subsequent exposure assessment.

The occurrence of patulin was investigated in 100 conventional and 69 organic fruity foodstuffs samples commercially available in Italy by using an HPLC method with a limit of quantification of 0.5 microg kg(-1). Patulin was detected in 26 (26%) conventional and 31 (45%) organic products with a significantly higher (p<0.01) mean concentration in the organic products (4.78 vs. 1.15 microg kg(-1)). Mean patulin concentrations in conventional apple juices, pear juices, other juices and fruits purees were 3.14, 0.22, 0.19, 0.11 microg kg(-1), respectively, and 7.11, 11.46, 2.10, 0.18 microg kg(-1) in the relevant organic products. Four samples of juices (one conventional and two organic apple, and one organic pear) contained patulin at concentrations above the limit of 50 microg kg(-1), four at concentrations between 10 and 25 microg kg(-1), and the remaining ones below 10 microg kg(-1). Patulin was detected (<1 microg kg(-1)) in only three of the 23 fruity baby food samples tested (homogenized fruits, 11 conventional and 12 organic). Based on the available data on Italian intakes of fruit juices, the estimated daily intakes of patulin, were 0.38 and 1.57 ng kg(-1) body weight (bw) from conventional and organic products, respectively. Estimated daily intakes of patulin for children were higher, 3.41 ng kg(-1) bw from conventional and 14.17 ng kg(-1) bw from organic products, but largely below the provisional maximum tolerable daily intake (PMTDI) of 400 ng kg(-1) bw. Patulin was also found in two samples of organic apple vinegar (<5 microg kg(-1)) and in fresh apples with rotten spots (12 out of 24 samples) with maximum levels at 16,402 and 44,572 microg kg(-1) for conventional and organic apples, respectively.     

Application of a commercial immunoassay to the direct determination of insecticide imidacloprid in fruit juices

An ELISA was used to directly determine residual imidacloprid in fruit juices. Imidacloprid could be determined by only diluting samples without any pre-treatments such as filtration, centrifugation, and clean-up procedures. The ELISA enabled imidacloprid to accurately determine down to about 5 μg/L in apple and grape juice samples and down to about 20 μg/L in orange juice sample. Recovery and precision of the ELISA were evaluated by spiking fruit juice samples with imidacloprid in the 10–400 μg/L ranges. Coefficients of variation were lower than 20% in all cases, and average recoveries were 94.2%, 113.2%, and 104.2% for apple, grape, and orange juice samples, respectively. No false positive results were found. The results obtained with the proposed ELISA well correlated with the reference HPLC for each fruit juice sample (r > 0.99).     

Patulin in domestic and imported apple-based drinks in Belgium: occurrence and exposure assessment

Apple-based beverages are regularly consumed by adults and children in Belgium. They are locally produced or imported from other countries. The apples used as starting material for these productions are frequently contaminated by mycotoxin-producing moulds and damaged during transport and handling. The current study was undertaken to investigate whether patulin (PAT) is present in the industrial or handicraft-made apple juices and ciders consumed by the Belgian population and to assess the population's exposure to this mycotoxin through apple-based drinks. Belgian (n = 29) and imported (14) apple juices as well as ciders (7) were assayed for PAT by high-performance liquid chromatography with ultraviolet light detection. PAT was detected respectively in 79, 86 and 43% of these tested samples. However, no contaminated sample exceeded the safe level of 50 µg PAT l^-1. Levels of PAT contamination were comparable in Belgian and imported juice samples. The overall mean PAT concentrations were 9.0 and 3.4 µg l^-1 for contaminated apple juices and ciders, respectively. This study also indicates that there was no statistically significant difference in the mean PAT contamination between clear (7.8 µg l^-1) and cloudy (10.7 µg l^-1) apple juices, as well as between handicraft-made apple juices (14.6 µg l^-1) and industrial ones (7.0 µg l^-1). On the basis of the mean results, a consumer exposure assessment indicates that a daily intake of 0.2 litres apple juice contributes to 45% of the provisional maximum tolerable daily intake for a child of 10 kg body weight.     

Determination of ochratoxin A in organic and non-organic cereals and cereal products from Spain and Portugal

The objective of this work was to know the occurrence of OTA in organic and non-organic cereals and cereal products from Spain and Portugal. A method based on extraction with matrix solid phase dispersion (MSPD) using octylsilica (C₈) followed by liquid chromatography coupled with fluorescence detection (LC–FD) was used to determine OTA from the selected samples. Recoveries of OTA from the studied samples spiked at 10 ng/g level ranged from 78% to 89% with a standard deviation of 3.66. The limits of detection and quantification of this method were 0.05 and 0.19 ng/g, respectively. Furthermore, LC–FD after OTA methylation was used to confirm the identity of OTA in all positive samples. This procedure was applied to 83 organic and non-organic samples including rice, wheat, barley, rye, oats and maize from Spain and Portugal. OTA was detected in 22% of the samples, with concentrations ranging from 0.20 to 27.10 ng/g. From the total OTA contaminated samples (n = 18), 72% were organic cereal and 28% were non-organic cereal samples, with mean concentrations of 1.64 and 0.05 ng/g, respectively. The 66% and 34% of contaminated samples were from Spain and Portugal, respectively, with mean concentrations of 0.93 and 0.64 ng/g for each country. Six contaminated samples exceeded the maximum limits (ML) for OTA fixed by European Commission Regulation (5 μg/kg), among them three were from Spain and three from Portugal.     

Processing and analytical characterisation of pulp-enriched cloudy apple juices

Pulp-enriched cloudy apple juices were manufactured from two apple varieties by blending of apple puree with natural cloudy apple juice in order to enrich bioactive secondary plant substances. Finishing of the puree with a 0.6-mm mesh screen and final product homogenisation revealed as the optimum processing technology for the novel 100% fruit beverage. The presence of large particles originating from the puree prevented long-term cloud stability, but due to the proportion of cloud-stable juice a complete phase separation did not occur. Optimal drinkability was achieved at a viscosity of 11.5 mPa s. Polyphenol compositions and concentrations were determined by means of RP-HPLC/PDA. The results ranged from 109 to 610 mg/l. All samples showed the typical polyphenol pattern of apples with dominating hydroxycinnamic acids followed by flavanols and flavonols. The puree addition to the cloudy apple juices increased the polyphenol concentrations by average 100%. Relatively, the highest increase could be observed for dimeric procyanidins. Different technological variants did not affect significantly the polyphenol concentrations. The dietary fibre contents of the pulp-enriched cloudy apple juices ranged from 5.8 to 9.4 g/l.     

A Fast and Reliable UHPLC-PDA Method for Determination of Patulin in Apple Food Products Using QuEChERS Extraction

A fast and reliable method for the quantification of patulin using ultra high performance liquid chromatography coupled to a photodiode array detector was developed and validated for the analysis of several apple-based foodstuffs. Sample preparation was based on the QuEChERS procedure. Samples were extracted with acetonitrile and partitioned with a mixture of sodium citrate, NaCl, and Mg₂SO₄. The cleanup step was performed using dispersive SPE mixed with Mg₂SO₄ and PSA. This step was carried out twice in order to improve chromatographic results. The method was validated in spiked cloudy apple juice, apple puree, apple yogurt, beer with apple juice, and cider and applied to 24 commercial samples. The limits of detection and limits of quantification were ≥0.4 and ≥2 ng/g, respectively. Both were below the maximum legal limit established by the European Union. Recoveries for all the matrices were between 78.4 and 94.7 % while relative standard deviations were between 3.8 and 10.4 %. Patulin was detected on four apple juices from concentrate, one cloudy apple juice from an eco-store, and one beer. Nevertheless, the highest concentration found was 25.4 ng/g.     

Polycyclic aromatic hydrocarbons (PAHs) in sugarcane juice

Sugarcane juice is a common beverage in many Brazilian cities. At harvesting season most sugarcane plantation is burnt and this procedure has been shown as an important source of PAHs emission. In the present study 80 samples of sugarcane juice collected from two Brazilian cities, in two different periods, were analysed for the presence of four PAHs: benz(a)anthracene, benzo(b)fluoranthene, benzo(k)fluoranthene and benzo(a)pyrene. PAHs were detected in 50% of the samples. The samples collected between harvests presented mean sums of PAHs of 0.013 μg/kg and 0.012 μg/kg, while the samples collected during harvest presented mean sums of 0.053 μg/kg and 0.055 μg/kg. A higher concentration and incidence of PAHs in the juices collected in the harvest period was verified, corroborating the burning of the crops as a source of sugarcane juice contamination.     

Classification of commercial apple juices based on multivariate analysis of their chemical profiles

Currently, a wide range of differently processed apple juices is available on the market. In this study the quality of commercial apple juices from four product categories was evaluated on the basis of their chemical profiles (total soluble solids, pH, titratable acidity, ratio of soluble solids to acidity, sugars, total phenolics content, and antioxidant activity) using multivariate methods. Principal component analysis has revealed, that the chemical parameters, such as titratable acidity, ratio of soluble solids to acidity, and pH (PC1) and sugars and total soluble solids (PC2) appears to be the parameters most differentiating the samples. Five classes of juices with similar chemical composition were detected using hierarchical cluster analysis. The exploratory analysis of the overall chemical profiles revealed that the juices clear from concentrate, cloudy not from concentrate and freshly squeezed, were easily distinguishable due to their unique properties. In contrast, cloudy juices from concentrate showed properties similar to juices of other classes. The classification based on k-nearest neighbors method had high sensitivity and low classification error for clear juices from concentrate and cloudy not from concentrate. The classification failed for the cloudy juices from concentrate.     

Fumonisin level in corn-based food and feed from Linxian County,a high-risk area for esophageal cancer in china

The level of mycotoxin fumonisins in corn-based food and feed collected from Linxian County, a high-risk area for esophageal cancer in China, has been analyzed using high-performance liquid chromatographic coupled with evaporative laser scattering detector (HPLC-ELSD). A total of 104 corn kernel samples were obtained from local households, granaries, wholesale markets (central markets), and retail markets (stores and supermarkets). Fumonisin B₁ (FB₁) was detected in the samples from households, granaries, central markets, and stores, with a positive rate of 61.5%, 50%, 33.3%, and 17%, respectively. No fumonisin was detected in samples from the supermarket. The highest FB₁ levels (0.30–3.20 μg/g; mean, 1.42 μg/g) were found in samples from the granary, followed by household (0.25–1.80 μg/g; mean, 0.73 μg/g), central market (0.25–1.10 μg/g; mean, 0.51 μg/g), and store (0.22–0.34 μg/g; mean, 0.28 μg/g). Among the 80 corn kernel samples collected from local households, 18 of 24 (75.0%) moldy samples contained high levels of FB₁ (0.28–3.30 μg/g; mean, 1.58 μg/g), and 20 of 56 (35.7%) apparently healthy samples contained low levels of FB₁ (0.21–0.82 μg/g; mean, 0.46 μg/g). As the central market plays an important role in trade of corn-based food and feed in China, a total of 115 corn-based food and feed samples were collected from the local central market. The highest FB₁ levels (0.30–3.13 μg/g; mean, 1.50 μg/g) were found in feed, followed by unprocessed food (0.31–0.63 μg/g; mean, 0.47 μg/g) and processed food (0.21–0.28 μg/g; mean, 0.25 μg/g). The positive incidence of FB₁ in feed, unprocessed, and processed food were 53.6%, 33.3% and 17.9%, respectively. In conclusion, the results showed that corn-based food and feed from Linxian County contained low level of FB₁ (<2 μg/g) in general, but efforts should be made to control the fumonisin contamination in corn kernels stored in granaries and households.     

Determination of aflatoxin levels in nuts and their products consumed in South Korea

A total of 85 nuts and their products marketed in South Korea were assessed for aflatoxins using a monitoring scheme consisting of enzyme-linked immunosorbent assay (ELISA) for rapid screening, high performance liquid chromatography (HPLC) for quantification and LC–mass spectrometry (MS) for confirmation. Thirty-one out of 85 samples gave ELISA readings above 0.06 and were screened as possible positive samples. Aflatoxin contents of possible positive samples were determined using HPLC with a detection limit of 0.08–1.25 μg/kg and a quantification limit of 0.15–2.50 μg/kg. Nine samples including 1 raw peanut, 4 roasted peanuts, 2 peanut butters, 1 pistachio and 1 seasoned assorted nut were contaminated with aflatoxins (10.6% of incidence), ranging in various levels up to 28.2 μg/kg. LC–MS analysis on contaminated samples revealed that peaks eluting at 4.4, 5.2, 9.1 and 11.9 min were confirmed as aflatoxin G₁, aflatoxin B₁, aflatoxin G₂ and aflatoxin B₂, respectively.     

Patulin in fruit juices: occurrence,bioaccessibility, and risk assessment for Serbian population

This paper reports the first study of patulin occurrence in fruit juices and risk assessment related to patulin intake by children, adolescents and adults in Serbia. During 3 consecutive years (2013–2015), 142 fruit (apple or multi-fruit) juices were collected from the market and analysed using HPLC-UV. Patulin was found in 51.4% of juices with 0.7% of the samples in excess of the legal limit of 50 μg kg^?1 (mean 4.3 μg kg^?1). Apple juices showed significantly higher percentage of contaminated samples (74.0% vs 27.5%), as well as higher mean patulin content (6.4 vs 2.1 μg kg^?1) when compared with the multi-fruit ones. Bioaccessibility of patulin in fruit juices was studied using the standardised in vitro digestion method. A mean of 21.6% of the initial patulin amount reached the end of the intestinal phase showing a significant reduction of this toxin during the human digestion process. Risk assessment of patulin intake by Serbian children, adolescents and adults, conducted by deterministic and probabilistic approaches and including the bioaccessibility results, revealed no health concern. Although patulin alone does not represent risk, further research should consider its co-occurrence with other toxic substances in food and potential adverse effects of their mixtures.     

Quantification of coumarin derivatives in Noni (Morinda citrifolia) and their contribution of quenching effect on reactive oxygen species

The quantification of coumarin derivatives such as scopoletin, 7-hydroxycoumarin (7-HC) and 4-hydroxycoumarin (4-HC) in Noni (Morinda citrifolia) was described. The coumarin derivatives were determined by HPLC-UV or -fluorescence detection. More than 95% of peak purity for coumarin derivatives in Noni sample was confirmed by a multi-wavelength fluorescence detector. Amounts of scopoletin and 7-HC in Noni juices (A–H) were ranging 5.1–231 μg/ml and 0.04–0.45 μg/ml, respectively (n = 12). No 4-HC was detected in any Noni samples examined.     

Patulin reduction in apple juice from concentrate by UV radiation and comparison of kinetic degradation models between apple juice and apple cider

Patulin, a mycotoxin produced by several genera of fungi, including Byssochlamys, Aspergillus, and Penicillium, has been an important concern in apple cider and apple juice due to its toxicity and health consequences. In this study, the effects of UV on the patulin level, physical and chemical properties, and sensory attributes in apple juice from concentrate were investigated. Kinetic modeling of patulin reduction by UV radiation in apple juice from concentrate was calculated and compared with the degradation rate observed previously in apple cider. From an initial patulin contamination of approximately 1,000 ppb (μg/liter), the UV exposure, ranging from 14.2 mJ/cm(2) (one pass) to 99.4 mJ/cm(2) (seven passes), was successful in reducing patulin levels by 72.57% ± 2.76% to 5.14% ± 0.70%, respectively. Patulin reduction by UV radiation followed first-order kinetic modeling in a fashion similar to first-order microbial inactivation. An exponential correlation between UV exposure and the percentage of patulin remaining was observed, giving an r(2) value of 0.9950. Apple juice was repeatedly exposed to 14.2 mJ/cm(2) for each treatment, and patulin levels were significantly decreased when compared with the level obtained with the previous UV exposure treatment. While there were no significant differences in the percentages of titratable acidity and ascorbic acid (P > 0.05), there were minor yet random sampling differences in pH and degrees Brix (1 °Brix is 1 g of sucrose in 100 g of solution; the °Brix represents the soluble solids content of the solution as percentage by weight [%, wt/wt]) (P ≤ 0.05). A significant difference (P ≤ 0.05) in sensory perception for the finished apple juice was detected between the control and the full seven-pass UV radiation treatment using an experienced consumer panel and a triangle test. Patulin reduction by UV radiation from both the current study and a previous study involving apple cider was compared, which showed that both matrices strongly fit a first-order kinetic degradation model. However, the kinetic constant for degradation in apple juice was approximately 5.5 times greater than that observed in an apple cider matrix.     

Aflatoxins contamination in spices and processed spice products commercialized in Korea

A survey for total aflatoxins (aflatoxins B₁, B₂, G₁, and G₂) was conducted on 88 spices and processed spice products commercialized in Korea. The presence of aflatoxins was determined by high-performance liquid chromatography (HPLC) with fluorescence detector using immunoaffinity column clean-up. Total aflatoxins (AFs) are detected in 12 samples (13.6% of incidence) including seven red pepper powder, two red pepper pastes (Kochujang), two curry and one ginger product. The contamination levels are 0.08–4.45 μg/kg as aflatoxin B₁ and 0.08–4.66 μg/kg as AFs. The liquid chromatography–tandem mass spectrometry (LC–MS/MS) analysis on contaminated samples was conducted for the confirmation of detected aflatoxins. The 12 samples which showed aflatoxins by HPLC/FLD were confirmed as aflatoxins by LC–MS/MS.     

Contamination of food products with patulin

Based on the method for patulin determination designed by the authors the rate and level of contamination of fruit, vegetables and foods manufactured from them (juices, purees, jams) with this mycotoxin were studied. Patulin was found in 8 out of 160 samples of fruit and vegetables, the highest concentration of patulin was identified in the berries of sea buckthorn (up to 54 000 micrograms/kg). Patulin was found in 28 out of 185 samples of foods manufactured from fruit. The concentration of patulin in juices did not exceed the allowable concentrations on the average. Patulin was largely identified in apple, sea buckthorn and plum juices.     

Comparative study of polyphenolic content and antiradical activity of cloudy and clear apple juices

Clear and cloudy apple juices from Idared and Champion varieties were studied for their radical‐scavenging effects. The polyphenolic content and composition of the juices before and after thiolysis were determined by high‐performance liquid chromatography with diode array detection. Cloudy juices, especially that prepared from Champion variety, had a higher content of procyanidins than clear juices. Radical‐scavenging activity was measured by electron paramagnetic resonance (EPR) spectroscopy using the stable 1,1‐diphenyl‐2‐picrylhydrazyl (DPPH) radical. All juices showed long‐lasting radical‐scavenging activity, and EPR spectra were recorded over time to follow the reaction kinetics. Scavenging of DPPH showed pseudo‐first‐order kinetics, which might be expected in the presence of polymerised antioxidants that prevent closer contact between the DPPH radical and hydroxyl groups. The content of polymeric procyanidins showed a linear dependence on the rate constant, suggesting that these compounds are mainly responsible for time‐extended radical‐scavenging activity. The antioxidant properties of apple juices were much better reproduced by EPR spectroscopy than by UV–visible measurements. The former method is especially sensitive to the concentration of polymerised or bound procyanidins, whilst the latter method requires transparent (clear) samples. Apple juices, especially cloudy ones, are a rich source of natural antioxidants that may be used in the pharmaceutical or food industry. Copyright © 2006 Society of Chemical Industry