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Senna, a medicinal herb, is highly susceptible to aflatoxin contamination, which often limits the export value of the final products due to the regulatory limits of importing countries. Presence of aflatoxin B1 (AFB1) was investigated in 229 senna pod samples at various stages from field to storage over three years. Higher incidence of AFB1 was revealed during the late harvest stage with a mean level of 52.4 µg/kg and a range of LOD-206 µg/kg. Out of 48 late harvest samples, 37 exceeded the AFFB1 limit of 2 µg/kg. In contrast, the majority of preharvest samples showed lower levels of AFB1 (1.0 µg/kg). During drying, increase in the mean AFB1 level to 4 µg/kg was observed and it could further increase to 18.1 μg/kg in storage. These results highlight the status of aflatoxin contamination in senna pods and emphasise the importance of implementing good agricultural practices in senna cultivation to mitigate AFB1 contamination. [ABSTRACT FROM AUTHOR]

Aflatoxin (AF) poisoning of staple foods, such as rice, is caused by fungal contamination by Aspergillus species. These AFs are genotoxic, carcinogenic and suppress the immune system. Hence, the present study was conducted to elucidate the prevalence of AF contamination in rice samples collected from local markets of Hyderabad, Telangana, India. The rice samples collected were analysed for AF by using HPLC-fluorescence detection (HPLC-FLD). Based on AF contamination levels and dietary intake of rice, the health risk was assessed by the margin of exposure (MOE) and liver cancer risk in adults, adolescence and children. The percentage detected contamination with AFB1 and AFB2 of rice samples was 54% and 34%, with the concentration ranging between 0–20.35 µg/kg and 0–1.54 µg/kg, respectively. Three rice samples exceeded the Food Safety and Standards Authority of India (FSSAI) total AF acceptable limit of 15 µg/kg. The average MOE values were 53.73, 50.58 and 35.69 (all <10,000) for adults, adolescence and children, respectively. The average liver cancer risk associated with rice consumption in the population of Hyderabad was found to be 0.27, 0.28 and 0.40 hepatocellular carcinoma (HCC) cases/year/100,000 individuals in adults, adolescence and children, respectively. This study revealed an adverse health risk to population of Hyderabad due to consumption of AF contaminated rice. [ABSTRACT FROM AUTHOR]

The natural co-occurrence of aflatoxins (AFs) and ochratoxin A (OTA) in liquorice roots obtained from different herbal outlets of Karachi, Pakistan, was evaluated. A total of 60 samples were obtained during 2019‒2021 and analysed using HPLC with fluorescence detection. The method was validated according to the European Union (EU) regulation. The incidence of AFs was 52 in all tested samples (87%), with a contamination range of 1.2‒6.4 µg kg−1 and an average of 2.1 ± 0.3 µg kg−1. In all samples, the AFs contamination was below the maximum limit (ML) of 10 µg kg−1 for total AFs as set by the EU. The OTA contamination in all samples ranged 1.5‒60.3 µg kg−1, with a mean of 18.9 ± 0.8 µg kg−1. In 36 samples (60%) the OTA contamination was below the ML of 20 µg kg−1 as set by the EU. These results led to the recommendation to test liquorice root on mycotoxins, as it comes to food quality standards. [ABSTRACT FROM AUTHOR]

Contamination of ochratoxin A (OTA) is a common concern for the quality and safety of licorice and its derivatives, while their complex sample matrices always restrict the monitoring and regulation of OTA. Taking the much more concentrated and complicated licorice extract as the representative, a modified analysis method was established for OTA by HPLC. Parameters were comprehensively investigated based on liquid-liquid extraction and immunoaffinity column clean-up. In comparison to other methods, the developed method achieved effective clean-up efficiency and selectivity without tedious procedures and specialized instrumentation. Good linearity (R2 ≥0.9995), low LOD/LOQ (0.10 μg/kg/0.33 μg/kg), and satisfactory recovery (90.0%-96.4%, RSDs <7.0%) indicated the satisfactory sensitivity and reliability of the method. In addition, the applicability and robustness of the method was demonstrated by the analysis of large numbers of licorice extract samples. It is noteworthy that 66.5% of 176 samples were contaminated with OTA, while the concentrations of 9.1% of samples exceeded the maximum limit (ML, 80 μg/kg) defined by the EU. On account of the high contamination frequency and broad concentration range of OTA, the daily intake limit of licorice extract was preliminarily determined to be 123.18–123.93 g/day (chronic exposure) and 24.24 g/day (acute exposure), indicating a potential of acute risk through daily exposure. This calls for improved supervision and regulation for OTA contamination in licorice samples. This study suggests a prospective option for the efficient determination and routine monitoring of OTA in licorice and its derivatives, simultaneously providing a valuable data base for its health risk assessment. [ABSTRACT FROM AUTHOR]

Colistin, in the form of colistin methanesulfonate sodium (CMS), has a narrow therapeutic window, and colistin levels must be monitored during treatment. The aim of this study was to develop and validate a high-performance liquid chromatography-fluorescence detection (HPLC-FLD) method for measuring colistin in human serum. Colistin was extracted from human serum using trichloroacetic acid and methanol for protein precipitation, followed by in-solid phase extraction derivatization with 9-fluorenylmethyl chloroformate. HPLC-FLD system using a reverse-phase HPLC C18 column and a mobile phase consisting of acetonitrile, tetrahydrofuran, and water (80%:4%:16%) were used for the quantification of colistin A, colistin B, and polymyxin B (internal standard) in human serum. The extraction recoveries were between 71% and 103%. Linear calibration curves were obtained for colistin in concentrations from 0.3 to 8.0 μg/mL, with good fit (r2 = 0.9993). The lower limit of quantitation was 0.3 μg/mL. The intra- and inter-day precision of the assay was 0.5–5% and 3.5–9.4%, respectively. The accuracy ranged from 98% to 100%. This validated method was successfully applied to the analysis of serum-receiving CMS in critically ill patients. This method will be useful to assist colistin dosage adjustment based on individual blood colistin levels for optimization of colistin therapy. [ABSTRACT FROM AUTHOR]

Thermal treatment of protein-rich food can lead to the formation of biologically active heterocyclic aromatic amines (HAAs). One of the methods to learn how to reduce the content as well as the influence of these compounds on heath is the study of factors inhibiting their synthesis. In the current investigation, the effect of onion and garlic on the formation of six possibly carcinogenic non-polar HAAs (α-, γ- and δ-carbolines) and two co-mutagenic β-carbolines (harmane and norharmane) was evaluated by comparing their contents in meat and gravy samples obtained from pan-fried pork dishes prepared in the presence and absence of these vegetables. Carbolines were isolated from food samples by solid phase extraction. The quantitative analysis was performed by high-performance liquid chromatography with fluorescence detection. The concentrations of individual compounds in dishes prepared without added vegetables ranged from 0.02 ng g−1 (3-amino-1,4-dimethyl-5 H-pyrido(4,3-b)indole; Trp-P-1) to 10.1 ng g−1 of meat (2-amino-9 H-pyrido[2,3-b]indole; AαC). Onion (30 g/100 g of meat) and garlic (15 g/100 g of meat) lowered the total content (in meat and gravy) of the α-, δ- and γ-carbolines in the range from 52% to 87%. In contrast, onion caused an increase in the norharmane concentration both in meat and gravy. The percentage of carbolines in the gravies (assuming that their total content in meat and gravy is 100%) was higher in dishes prepared with onion and garlic than in dishes without these seasonings. [ABSTRACT FROM AUTHOR]

Large-scale food fortification of vegetable oils with vitamin A has been implemented successfully for decades in numerous African and Asian countries, contributing demonstrably to reductions in vitamin A deficiency. For these programmes, reliable and validated analytical data are essential to demonstrate compliance with legal standards and fortification levels. Commonly, many analytical laboratories use a saponification method for the quantitative analysis of retinyl palmitate (the mostly used form of vitamin A for fortification) in fortified oils, which implies a multiple-step procedure with long analysis times and the potential risk of analyte loss. The aim of the present study was to develop and validate a direct High-performance Liquid Chromatography (HPLC) method that reduces these sample preparation steps, leading to the cost- and time-efficient quantification of retinyl palmitate in fortified oils. Oil samples are dissolved into the HPLC solvents, then injected directly into a common C18 column, and subsequently detected by a fluorescence detector. The limit of quantification (1.0 mg retinyl palmitate kg−1) and the working range of 1.0–100 mg retinyl palmitate kg−1 with a linearity of R2 = 0.9989 are appropriate to analyse fortified oil samples. The method also showed adequate precision (RSD between 1.1% and 3.1%) and recoveries (86–103%) at two different concentration levels. The accuracy of the direct HPLC method was additionally proven by the comparison of spiked samples with two external laboratories that used the saponification method. The robustness of the method was confirmed by the analysis of various spiked edible oils. The HPLC column is not deteriorated by the lipid matrix and shows excellent stability and long lifetime. Also, 9-cis-retinyl palmitate formed mainly by light exposure could be detected by this method. The direct HPLC method is a well-suited alternative to the saponification method for the rapid and reliable routine analysis of fortified oil samples. [ABSTRACT FROM AUTHOR]

Urea is authorised in the European Union (EU) as feed additive for ruminants. Because of its high molecular nitrogen content, it is a substance for potential protein adulteration in non-ruminant feed. The EU defines a spectro-colorimetric method as an official control method for the determination of urea in feed, whereas the Association of Official Analytical Chemists (AOAC) in the United States recommends an enzymatic method. Discrepancies between results obtained by these different approaches have been reported, especially at low concentrations. Therefore, we developed and validated two methods for urea determination in compound feed, including pet food, and yeast (Saccharomyces cerevisiae) over a wide concentration range using high-performance liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) and fluorescence detection (HPLC-FLD) and compared performance with a commercial enzyme kit. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 3 and 8 mg kg−1 for LC-MS/MS and 2 and 7 mg kg−1 for HPLC-FLD, respectively. For both methods, the variation coefficients ranged between 1.4% and 7.2% in ruminant feed used as reference material as well as spiked samples of complete feed for chicken, pet food for dogs and cats, as well as yeast. Recovery rates for spiked samples ranged from 86% to 105%. For real samples of complete feed for poultry, wet and dry pet food for cats and dogs and yeast amounts of urea between < LOD and 200 mg kg−1 relative to a feedingstuff with a moisture content of 12% were found. In comparison with the enzyme kit, the newly developed methods proved to be less time-consuming in sample preparation and more stable regarding matrix effects. [ABSTRACT FROM AUTHOR]

Atmospheric contamination of plant raw material with Polycyclic Aromatic Hydrocarbons (PAHs) helps explain their presence in edible vegetable oils. This study compared PAH contamination of Turkish olive fruits during their growing period on the tree and their respective oils from three different industrial sources (petroleum refinery, thermal power plant and heavy industry site). The method included liquid-liquid extraction solid-phase extraction for cleanup followed by HPLC with fluorescence detector. There were statistically significant differences between the three industrial sources in benzo[a]pyrene content, the sum of light, total PAHs and PAH4 (p˂0.05), but only slight differences in PAH profiles. The highest level of PAH compounds was measured in samples exposed to pollution from the petroleum refinery, nearly twice as high as samples exposed to the thermal power plant which showed the lowest contamination levels. None of the samples analysed exceeded the limits stipulated by current legislation. The transfer ratios of PAH compounds from olives to olive oil were 22.8–73.2%. This indicates that PAHs either diffuse directly from skin to oil within the fruit or transfer during oil extraction. [ABSTRACT FROM AUTHOR]

In this study, the effect of three essential oils (EOs) – clove oil (CO), thyme oil (TO), and garlic oil (GO), which are generally recognized as safe – on the planktonic growth, minimum inhibitory concentration (MIC), minimum bactericidal concentration (MBC), motility, biofilm formation, and quorum sensing (QS) of Vibrio parahaemolyticus was investigated. All three EOs showed bacteriostatic activity, with MICs in the range 0.02%–0.09% (v/v). CO and TO completely controlled planktonic growth at 0.28% and 0.08% (v/v), which is four times their MIC (4 × MIC), after 10 min, whereas GO completely controlled growth at 0.36% (v/v) (4 × MIC) after treatment for 20 min. V. parahaemolyticus motility was significantly reduced by all three EOs at 4 × MIC (0.28% for CO, 0.08% for TO, and 0.36% for GO), whereas QS was controlled and biofilm formation reduced by all three EOs at 8 × MIC (0.56% for CO, 0.16% for TO, and 0.72% for GO) after 30 min of treatment. These results suggest that CO, TO, and GO have a significant inhibitory effect on V. parahaemolyticus cells in biofilm sand thus represent a promising strategy for improving food safety. These results provide the evidence required to encourage further research into the practical use of the proposed EOs in food preparation processes. [ABSTRACT FROM AUTHOR]

Infestation of food crops by fungi has led to serious economic losses in the international market. There is a paucity of information on the multi-mycotoxin profile of cashew nuts from different geographical locations in Nigeria and South Africa. This work aims at comparing the fungal metabolite profile of cashew nut from two African countries using HPLC-FLD and LC-MS/MS. The differences in distribution of the fungal metabolites across the two countries were also examined. A total of 75 (39; Nigeria, 36; South Africa) roasted cashew nuts were purchased from 14 different locations in Nigeria and 10 major supermarkets in South Africa. The samples were subjected to HPLC analysis for aflatoxin and zearalenone and LC-MS/MS analysis for multiple metabolite profiling. Total aflatoxins (0.03-0.77 µg/kg and 0.01-0.28 µg/kg) and zearalenone (123.2 and 788.6 µg/kg) were quantified in nut samples from South Africa and Nigeria, respectively. In contrast, LC-MS/MS analysis showed that none of the major fungi metabolites except for one (citrinin) was present in detectable amount in Nigerian cashew nuts (31.3 μg/kg). Other microbial metabolites present in the nuts were; Aspergillus metabolites (< LOD to 398 × 104 μg/kg and < LOD to 1760 μg/kg); flavoglaucin (5.4-177.4 μg/kg and 45.5-18,368 μg/kg), 7-hydroxykaurenolide (5.5-45.8 μg/kg and 3.5-33.7 μg/kg), chloramphenicol (0.3-4.5 μg/kg) for South African and Nigerian cashew nuts, respectively. The incidence rate of the fusarium toxins beauvericin and bikaverin were higher in Nigerian cashew nut (100% and 17%) than the South African nuts (8% and 8%), 7-Hydroxykaurenolide and chloramphenicol were found in all the cashew nut samples. A total of 15 unspecific metabolites (17-100%) were recorded in the nuts from both countries. Information on the metabolite profile of cashew nuts will provide useful information for policy makers, border agencies and other health-related Institutes. Fungi metabolites profile of Cashew nut from selected locations in Two African Countries. *Roasted cashew nut image- [ABSTRACT FROM AUTHOR]

This survey describes the occurrence and levels of AFs and OTA in chocolate products consumed in Turkey. A total of 130 samples, including bitter chocolate, milk chocolate and chocolate wafers were analysed for these mycotoxins by high-performance liquid chromatography coupled with fluorescence detection (HPLC-FLD). The values of recovery (81–92%) and precision (RSD < 9%) fulfilled the requirements of EC Regulation No. 401/2006. OTA was the most prevalent mycotoxin, with an incidence of 46.7% in bitter chocolate, 22.8% in milk chocolate and 17.4% in chocolate wafers, ranging from 0.18 to 0.75 μg kg−1. AFs were detected in 13.3% of bitter chocolate, in 19.6% of milk chocolate and in 8.7% of chocolate wafers, in concentrations ranging from 0.15 to 2.04 μg kg−1. [ABSTRACT FROM AUTHOR]

Aflatoxin M1 (AFM1) is a 2B Group human carcinogens agent and introduces into the human diet by milk consumption. In the present study 257 raw, 143 pasteurized and 61 UHT milk samples were collected from markets in 117 cities throughout Iran, during winter 2017 and AFM1 contents were determined using a HPLC-FLD method after immunoaffinity clean-up. Mean recovery rates and relative standard deviations of the method were 90.6 ± 5.7%. AFM1 was detected in 252 of 461 (54.7%) samples (mean 31.3 ± 8.8 ng/L), ranging from <10 to 150 ng/L. Three samples (0.6%) exceeded the Iranian maximum limit of 100 ng/L. The mean AFM1 content was significantly higher in raw milk samples obtained from humid climate areas. The extrapolated concentration of AFB1 in dairy cattle feed based on the AFM1 value of milk was 1.96 µg/kg. The AFM1 contamination of milk seems not to be a serious public health concern in Iran. [ABSTRACT FROM AUTHOR]

Urinary aromatic diamines are exposure biomarkers of diisocyanate which are highly irritating to skin, mucosa and the upper respiratory system. In this study, a highly sensitive and selective high-performance liquid chromatography-fluorescence detection (HPLC-FLD) method was developed for determination of three aromatic diamines, 4,4′-methylenedianiline (MDA), 2,4-toluenediamine (4TDA) and 2,6-toluenediamine (6TDA) exposed to corresponding diisocyantes in human urine. The whole idea is based on an intramolecular excimer-forming fluorescence derivatization using 4-(1-pyrene)butanoyl chloride (PBC), followed by performing HPLC-FLD analysis.The resulting polypyrene-labeled derivatives of these aromatic diamines provided intramolecular excimer fluorescence at the emission wavelength of 475 nm wavelengths, which was shifted markedly to the higher emission wavelengths as compared with the wavelengths of the pyrene monomer. Under this condition, interferences such as amino acids and biogenic monoamines gave no peaks. It was found that using PBC derivatization, it was possible to improve the sensitivity and selectivity toward aromatic diamines. The limits of detection (LODs) were in the range of 0.30–0.52 ng/L, while the limits of quantitation (LOQs) between 1.05 and 1.63 ng/L. The intraday and interday precision was in the range of 3.6–4.5% and 4.1–5.7%, respectively. The proposed method was successfully applied to the quantitation of these exposure biomarkers in human urine samples. [ABSTRACT FROM AUTHOR]

An HPLC method with fluorescence detection has been developed and validated for the quantification of six fluorescent whitening agents (FWA) in plastic beverage cups after extraction and in food simulants after migration at 70°C for 2 h. The sensitivity of the method was high with LODs ranging from 0.053 to 0.251 μg kg−1 and LOQs from 0.107 to 0.504 μg kg−1. Accuracy and precision were highly acceptable, with recoveries greater than 82% and RSDs (%) below 16%. The expanded combined uncertainty was found to be less than 23% for the measurements of all studied FWAs. In extracting the analytes from food contact materials (FCM), accelerated solvent extraction (ASE) and Soxhlet extraction were applied using ethanol as the extraction solvent. The results obtained for FWA in 10 different food plastic cups, made from different polymers, were compared. The ASE technique proved to be faster, more effective and efficient than Soxhlet extraction. Migration tests with official food simulants from Regulation (EU) No 10/2011 showed that the substances studied could potentially migrate using the selected migration conditions. The most pronounced effect was observed in case of simulant D1 (50% w/v ethanol in water). The analytical method proved to be a simple, fast, sensitive and reliable tool for the simultaneous quantification of six of the most used FWAs in both FCM extracts and food simulants after migration experiments. [ABSTRACT FROM AUTHOR]

A total of 64 samples of sorghum (37 Tunisian sorghum samples and 27 Egyptian sorghum samples) were collected during 2011-2012 from markets in Tunisia. Samples were analysed for contamination with aflatoxin B1, ochratoxin A and zearalenone by High-Performance Liquid Chromatography Coupled with Fluorescence Detection (HPLC-FLD). Aflatoxin B1 was found in 38 samples in the range 0.03-31.7 µg kg−1. Ochratoxin A was detected in 24 samples with concentrations ranging from 1.04 to 27.8 µg kg−1. Zearalenone was detected in 21 samples and the concentration varied between 3.7 and 64.5 µg kg−1. ANOVA analysis of the influence of the country of origin on the incidence and concentration of mycotoxins in the samples studied showed no significant difference (P > 0.05) between the two batches of samples for each of the three mycotoxins studied. The studied mycotoxins contaminate sorghum and may also co-exist because of the diversity of the mycobiota in this cereal. [ABSTRACT FROM AUTHOR]

In recent years climate changes recorded in temperate regions of Europe have led to aflatoxin (AF) contamination of maize. Thus, the aim of this study was to investigate the influence of weather conditions on levels of aflatoxin B1 (AFB1), aflatoxin B2 (AFB2), aflatoxin G1 (AFG1) and aflatoxin G2 (AFG2) in 180 maize samples collected from the main maize-growing regions (Western Bačka, North Banat, South Banat and Central Serbia) in Serbia after harvest in 2015. The concentrations of AFs were determined by a validated HPLC method with post-column derivatisation and fluorescence detection (HPLC-FLD). The presence of AFB1, AFB2, AFG1 and AFG2 was detected in 57.2%, 13.9%, 5.6% and 2.8% of maize samples in the concentration ranges of 1.3–88.8 µg kg–1, 0.60–2.8 µg kg–1, 1.8–28.5 µg kg–1 and 2.1–7.5 µg kg–1 respectively. The recorded smaller amount of precipitation and especially higher air temperatures during the summer of 2015 were favourable for AF production, which resulted in 32.2% and 21.1% of samples being unsuitable for human consumption, since AFB1 and the sum of AFs concentrations were above 5.0 and 10.0 µg kg–1 respectively. Furthermore, the findings in this study indicate that the microclimate conditions in the investigated regions had a great influence on the contamination frequency of maize with AFs. The highest percentage of samples unsuitable for human consumption, considering both AFB1 and total AFs content were 72.5% and 51.5% respectively from Central Serbia, whilst the lowest percentages of 15.6% and 6.2% respectively were found in Western Bačka. These findings confirmed that maize should be continuously monitored in order to protect human and animal health from the harmful effects caused by AFs contamination. [ABSTRACT FROM AUTHOR]

In this research, 42 mesir paste samples produced by a limited number of manufacturers in Manisa, Turkey, were analysed for aflatoxin content by high-performance liquid chromatography with a fluorescence detector after pre-separation using immunoaffinity columns. A good correlation was found with good performance in terms of precision for the method. Limit of detection-limit of quantitation of AFG2-AFB2and AFG1-AFB1were 0.05/0.15 and 0.03/0.09 µg/kg, respectively. AFG2, AFG1 and AFB1were detected in 29%, 71% and 52% samples, whereas AFB2was not detected in any sample. AFtotal, AFG2, AFG1and AFB1content varied between 0.04/10.20 µg/kg, 0.07/0.42 µg/kg, 2.02/10.11 µg/kg and 0.04/0.11 µg/kg, respectively. About 9.5% of samples were found to be above the maxium limit (ML) for AFtotal(10 µg/kg), but none of samples exceeded the ML for AFB1(5 µg/kg) as set by the European Union for spices. According to the results, it was concluded that traditional products like mesir paste which contains different types of spices should be examined in terms of aflatoxins. [ABSTRACT FROM PUBLISHER]

Vibrio parahaemolyticusis an inhabitant of marine and estuarine environments and causes seafood-borne gastroenteritis in humans. In this study, an UltraFast LabChip Real-Time PCR assay was evaluated for rapid detection and quantification of pathogenicV. parahaemolyticusisolates.Escherichia coliandVibrio harveyiwere used as negative controls. Twenty-sixtdh-positive, biofilm-producingV. parahaemolyticusisolates were analyzed by repetitive extragenic palindromic-polymerase chain reaction (REP-PCR). REP-PCR analysis showed that the majority of theV. parahaemolyticusisolates originated from seafood and that clinical specimens formed two major clusters at 92.8% and 32% similarity levels. The presence and quantification of Autoinducer-2 was carried out using high-performance liquid chromatography with fluorescence detection (HPLC-FLD) after derivatization of Autoinducer-2 with 2, 3-diaminonaphthalene. The presence oftdh-positiveV. parahaemolyticusin marine samples highlights the need for constant environmental monitoring to protect public health. [ABSTRACT FROM AUTHOR]

A total of 225 maize kernel samples were collected from Shandong Province in China from 2012 to 2014 and analysed for contamination withFusariumspp. and fumonisins (FBs) using molecular methods and high-performance liquid chromatography with fluorescence detection. The results showed that the average incidences ofFusariumspp. in 2012, 2013 and 2014 were 23.3%, 37.1% and 36.5%, respectively,Fusarium verticillioidesbeing the predominant species. In 2012, the average contamination level of FBs was 3071 ng g−1, which was higher than that in 2014 (2913 ng g−1) and 2013 (2072 ng g−1). Of all samples, 13% and 19% had FB contamination levels higher than 2000 and 4000 ng g−1, which are the maximum limits as set by the Food and Drug Administration of the United States and the European Commission, respectively. Therefore, efforts should be taken to minimise the potential risk of FBs to the health of humans and animals. [ABSTRACT FROM AUTHOR]

This study aims to detect aflatoxins (AFs) in dairy cow feed, milk and milk products using a high-performance liquid chromatography coupled with fluorescence detection (HPLC-FLD) method. All the validation parameters met the method performance criteria of the European Union. The samples comprised 76 dairy cow feeds and 205 milk and milk products (including yoghurt and yoghurt-based beverage,ayran). AFs were present in 26.3% of the feed samples. Two feed samples exceeded the maximum limit (ML) of 5 µg kg−1for AFB1as established by the EU. Nineteen milk samples (21.1%) contained aflatoxin M1(AFM1) of which three exceeded the EU ML of 0.05 µg l−1. In addition, only two yoghurt samples and oneayransample contained AFM1, but the levels were lower than the EU ML. [ABSTRACT FROM PUBLISHER]

The aims of the present study were to investigate the occurrence of aflatoxin B1(AFB1), aflatoxin B2(AFB2), aflatoxin G1(AFG1) and aflatoxin G2(AFG2) in dairy cow feedstuff samples collected from four west provinces in Iran and estimate the corresponding concentrations of aflatoxin M1(AFM1) in milk during winter and summer in 2014. A total of 160 feed samples consisting of corn silage (n = 40), alfalfa hay (n = 40), straw (n = 40) and barley (n = 40) were analyzed using high-performance liquid chromatography with a fluorescence detector method. AFB1, AFB2, AFG1and AFG2were detected in 82.5%, 69.37%, 43.12% and 41.87% of the feed samples, respectively. The concentration of AFB1in 65% (26/40) and 10% (4/40) of corn silage and straw samples was higher than the European Union limit, respectively. Estimation of the total corresponding concentration of AFM1in milk was evaluated as 20.16 and 35.68 ng/l during summer and winter, respectively. [ABSTRACT FROM PUBLISHER]

The aim of this study was to investigate the presence of Ochratoxin A (OTA) in red pepper flakes commercialised in Turkey. A total of 75 samples were collected from different supermarkets and traditional bazaars in Istanbul during 2012–2013. OTA analysis was performed by high-performance liquid chromatography equipped with fluorescence detection after immunoaffinity column clean-up. The method was linear in the range 0.05–40 μg kg−1(r2 = 0.9997). Twenty-seven out of 31 (87.1%) packed red pepper flake samples contained OTA at concentrations ranging from 0.6 to 1.0 μg kg−1, whereas 100% of the unpacked red pepper flake samples contained OTA, in the range 1.1–31.7 μg kg−1. Overall, only 4 unpacked samples (5.3%) contained OTA, with a mean value of 23.4 μg kg−1, which is higher than the European Union limit. It is suggested that OTA content should be carefully considered in red pepper flake samples especially marketed in unpacked form. [ABSTRACT FROM PUBLISHER]

Aflatoxin M1(AFM1) occurrence was analysed in 80 samples of milk and 21 samples of infant formulae on the Serbian market, using high-performance liquid chromatography with fluorescence detection. All milk samples collected in 2013 showed AFM1 contamination in the range 0.02–0.32 μg kg−1, with a mean level of 0.13 μg kg−1. The EU maximum level for AFM1 in milk (0.05 μg kg−1) was exceeded in 75% of the samples. In 2014, AFM1 was found in 83%, 70%, 80% and 58% of the samples collected in April, July, September and December, respectively, exceeding the limit in 5% of the samples taken in July. The additional number of liver cancer cases per year associated with exposure to AFM1 was estimated to be 0.004 in the adult population. Regarding infant formulae, AFM1 was found in only one sample. [ABSTRACT FROM PUBLISHER]

Occurrence of aflatoxin M1 (AFM1) was determined in 254 samples of raw milk obtained from dairy cow farms of Qazvin Province, Iran. Aflatoxin M1 analysis was carried out by using the competitive enzyme-linked immunosorbent assay technique for screening and high-performance liquid chromatography with fluorescence detection for confirmatory purposes. The limit of detection and quantification of the confirmatory method were 0.003 and 0.01 µg/l, respectively. Aflatoxin M1 was detected in 204 analysed samples (80.3%), ranging from 0.011 to 0.321 μg/l, and 144 samples (56.7%) had levels above the Iranian national standard limit of 0.050 μg/l. Considering the seasonal variability, the occurrence and levels of AFM1 in samples obtained in winter were significantly higher (P < 0.05) than those obtained in summer. The results of this survey indicate the usefulness of a monitoring programme to supervise food safety for consumers. [ABSTRACT FROM AUTHOR]

A total of 85 walnut samples collected between October 2012 and April 2013 in different provinces of Turkey were analysed for the presence of aflatoxins (AFs). The method involved methanol–water extraction, clean-up with immunoaffinity columns and a sensitive high-performance liquid chromatography coupled with fluorescence detection after post-column derivatisation. The method was validated for selectivity, linearity, trueness, precision, limit of detection and limit of quantification (LOQ), which met the performance criteria as set by EC regulation No. 401/2006. LOQs were 0.07, 0.04, 0.09 and 0.05 µg kg–1for AFB1, AFB2, AFG1and AFG2, respectively. AFs were present in 9.4% of walnut samples (8/85) at total AFs levels ranging from 0.09 to 15.4 µg kg–1. Only one of eight walnut samples exceeded the European Union limit of 2 and 4 µg kg–1for AFB1and total AFs, respectively. [ABSTRACT FROM AUTHOR]

Ochratoxin A (OTA) is a mycotoxin that occurs in raw material and in several foods including meat and meat products. Cured ham may be contaminated by OTA directly forAspergillusandPenicilliumattack or indirectly as resulting from the carry-over of contaminated feeds to the edible tissues and organs of pigs. Due to OTA possible carcinogenic activity, the Italian Ministry of Health, took a precautionary measure, and a guideline value of 1 µg/kg of OTA in pork meat and derived products is in place. Analytical validated methods for the detection of OTA in meat products are required in order to comply with the guideline value and to respond to the official control requirements. Two validated methods are proposed, one based on high performance liquid chromatography fluorescence detection and one based on ultra performance liquid chromatography tandem mass spectrometry. The obtained data showed the strengths and also the limits of the two methods in terms of accuracy, limit of detection, and limit of quantification. The goal of this study was to identify the most suitable strategy for OTA determination in cured ham. [ABSTRACT FROM AUTHOR]

The presence of polycyclic aromatic hydrocarbons (PAHs) in Italian commercial milk samples is reported. The study was carried out on lactating (cow and goat) and plant (rice, soya, oat) milk. The quantitative determination involved liquid–liquid extraction of PAHs, a pre-concentration and determination by HPLC using a fluorescence detector. The recovery of analytes was in the range of 70–115%. The precision of the method was found to be between 6% and 24%. The detection limit ranged from 0.66 to 33.3 µg l–1corresponding to 0.03–1.66 µg kg–1milk (wet weight), at a signal-to-noise ratio of 3, depending on the compound. By this procedure, the levels of more volatile PAHs (two to three aromatic rings) were confirmed in 34 commercial milk and three plant milk samples, whereas benzo[a]pyrene was found only in five pasteurised milk samples at a mean concentration of 0.17 µg kg–1milk. These results provide evidence that PAH levels are influenced by heat treatments and skimming processes of milk production. [ABSTRACT FROM PUBLISHER]

Context: Few methods have been reported for the quantification of ligustilide (LIG) in biosamples: the pretreatment of the biological samples were laborious and time-consuming. Objective: A high-performance liquid chromatographic method with fluorescence detection (HPLC-FLD) for the determination of LIG in rat plasma was developed and validated. Pharmacokinetics and bioavailability of LIG were determined by systematic investigation in Sprague-Dawley rats. Materials and methods: LIG was isolated from the volatile oil of Radix Angelica sinensis and further purified by silica gel column chromatography. Podophyllotoxin was used as an internal standard. The analytes were detected by using fluorescence detection at an excitation and emission wavelength of 290 and 395 nm during 0-4 min, and 336 and 453 nm during 4-14 min, respectively. LIG pharmacokinetics was studied in rats after oral and intravenous administration of 12.5, 25 and 50 mg/kg doses. Results: Two calibration curves ( Y = 133.49 X − 14.27 ( r = 0.9995), Y = 145.61 X + 13.76 ( r = 0.9996)) were constructed in the range of 2.44-10 000 ng/mL for LIG with a lower limit of quantitation of 2.44 ng/mL. Both intra-day and inter-day precision were less than 6%. Accuracy ranged from 88.93 to 99.52%. The recovery ranged from 89.07 to 99.71%. The absolute bioavailability values were 71.36, 68.26 and 75.44% for oral doses of 12.5, 25 and 50 mg/kg, respectively. Conclusion: The present HPLC-FLD method was rapid, sensitive and reliable. LIG was absorbed and eliminated rapidly in rat. [ABSTRACT FROM AUTHOR]

A simple and sensitive HPLC method with fluorescence detection (HPLC-FLD) is reported for the simultaneous determination of metabolites of four nitrofuran drugs (furazolidone, furaltadone, nitrofurantoin and nitrofurazone) in pork muscle. The method involves acid hydrolysis of the protein-bound drug metabolites and the conjugation of the released side-chains with a novel fluorescence agent 2-hydroxy-1-naphthaldehyde. After liquid–liquid extraction and effective separation of the derivatives on a YMC-Pack Polymer C18 column at 40°C under alkaline conditions, the high fluorescence intensity of these derivatives at emission wavelengthλem = 463 nm enables their simultaneous determination in pork muscle at concentrations as low as 1 µg kg−1. The method was validated using blank pork muscle fortified with all four metabolites at 0.5, 1.0 and 2.0 µg kg−1. Recoveries were > 92.3% with RSDs < 8.5% for all four metabolites. The results obtained with HPLC-FLD and LC-MS/MS methods showed very good agreement for pork muscle samples. [ABSTRACT FROM PUBLISHER]

Ochratoxin A (OTA) is a naturally occurring mycotoxin and widespread food contaminant which results in a probable human exposure. A total of 85 samples (50 dried grapes, 10 grape juices and 25pekmez(boiled and concentrated grape juices) were collected from different supermarkets and traditional bazaars in Istanbul during 2008–2009. An analytical method based on immuno-affinity column for clean-up and high-performance liquid chromatography equipped with fluorescence detection was used to determine the OTA. Contamination frequencies were 8%, 20% and 88% with mean concentrations of positive samples of 1.15, 1.40 and 2.04 µg/kg for dried grapes, grape juices andpekmezsamples, respectively. These levels were lower than the maximum levels as set by the European Commission (EC). However, 12 of 25pekmezsamples had higher levels than permitted by the European Union (EU) for safe consumption. [ABSTRACT FROM AUTHOR]

Wolfberry fruit wine (WFW) is widely used as a global functional food to improve the immune system and prevent human disease. A total of 36 bottled WFWs were randomly collected in China between 2005 and 2010. Samples were analysed for the presence of ochratoxin A (OTA) using immunoaffinity column (IAC) clean-up and high-performance liquid chromatography with fluorescence detection (HPLC-FLD). Positive results were confirmed by liquid chromatography–electrospray ionisation–tandem mass spectrometry (LC-ESI-MS/MS). The limit of detection (LOD), based on a signal-to-noise ratio of 3, was 0.05 ng mL–1. Recoveries ranged from 78.3% to 94.7% and relative standard deviations from 1.1% to 4.3% within the spiking range of 0.2–20 ng mL–1. OTA was detected in one sample, below the maximum allowable limit as established by the European community. [ABSTRACT FROM AUTHOR]

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

Some polycyclic aromatic hydrocarbons (PAHs), particularly those with a high molecular mass, have been classified as probably being carcinogenic to humans by the International Agency for Research on Cancer (IARC). The significance of the determination of PAHs is reflected by the special attention the European Union is paying to regulating their maximum allowed levels in various types of foodstuffs. Like tobacco and smoked meats, alcoholic drinks can also contain these carcinogenic chemicals, as the latter have been detected in the charred insides of barrels, some ingredients such as caramel or the smoke released during the drying of germinated barley in beer or whisky. This paper determined the contents of seven PAHs in alcoholic beverages of variable alcoholic strength that had been aged in charred barrels for different times (months, years). The aim was to elucidate the dependence of the formation of seven PAHs on the type of charring (traditional or convective) used and the charring intensity (light, medium or heavy). Based on the results, the way the tree raw material is toasted strongly influences PAH levels in alcoholic drinks; thus, traditional charring produces increased amounts of PAHs from the wood relative to convective toasting. The sum of the analysed PAH concentrations in the aged alcoholic beverages studied ranged from zero for a white wine to 172&ThickSpace;ng l –1 for a ‘brandy de jerez solera’. The carcinogenic indicator benzo[ a ]pyrene was found at concentrations below 10&ThickSpace;ng l –1 . These PAH concentrations in alcoholic beverages are very low relative to those in smoked and char-broiled foodstuffs. Any health hazards, however, can be minimized by using convective toasting to manufacture the barrels where the drinks are to be aged. [ABSTRACT FROM AUTHOR]

Polycyclic aromatic hydrocarbons (PAHs), at least those with high molecular mass, are classified as probable human carcinogens by the US Environmental Protection Agency. The importance of the material used to generate smoke is indicated by the attention that the European Union is paying to list the wood that can be used to produce smoking flavour agents. The paper examines the dependence on the nature of the wood used for smoking on the formation of eight PAHs (selected as markers of PAHs) and transfer of these PAHs into traditional Spanish smoked chorizo sausages with collagen and tripe casings. The results showed that the kind of combustion performed on different materials seriously affected the PAH levels in the smoke generated. Ignition and firing of the material with a flame compared with heating produced more PAHs in the smoke. The levels of PAHs found in the meat and in the collagen and tripe casings of the smoked chorizo samples suggest that the collagen-based casings behave as a better barrier to PAHs. [ABSTRACT FROM AUTHOR]

A new analytical method was developed for the routine specific determination of the anionic surfactant Alcohol polyEthoxylate Sulfate (AES) in environmental aqueous samples. An enrichment/fractionation of the target analytes in water samples was performed by solid-phase extraction (SPE) on graphitized carbon black (GCB) (recoveries: 90-103%), followed by hydrolysis/derivatization with fluorescent reagents and separation/detection by reversed-phase high performance liquid chromatography coupled with fluorescence (HPLC-FLD). The developed procedure was applied to the study of the aerobic biodegradation of AES under laboratory conditions and to a ten-month monitoring of AES, as well as of linear alkylbenzene sulfonates (LAS), nonylphenol polyethoxylates (NPE) and alcohol polyethoxylates (AE) surfactants, in the Po river (Northern Italy). The residual concentrations found in the river waters were compared and used for a preliminary estimation of the annual average loads of monitored surfactants in the Adriatic Sea. [ABSTRACT FROM AUTHOR]

A sensitive and robust HPLC method with fluorescence detector (FLD), photochemical reaction device (PHRED) was developed to determine Aflatoxins (B1, B2, G1, and G2) and Ochratoxin A in animal feeds. Immunoaffinity columns (IAC) was used to purify the samples. According to monitoring resulted with the established method, aflatoxin and ochratoxin A were found in 44 of 496 domestic commercial samples (8.9% detection rate) and the concentration ranges were 1.76–162.69 μg/kg for Aflatoxin B1, 23.01–45.42 μg/kg for Ochratoxin A in 2015. In 2016, % detection rate was 22.2% (115 of 518 samples) and the concentration ranges are 1.76–43.69 μg/kg for Aflatoxin B1, 3.38–15.80 μg/kg for Ochratoxin A. The developed method was specific and reliable and is suited for the routine analysis of aflatoxin in animal feed. [ABSTRACT FROM PUBLISHER]