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Determination of aflatoxins as a group of potent contaminations in many food products is a common analysis in food quality control laboratories. For quantification of the four most toxic aflatoxins (AFs) (i,e. AF B1, B2, G1, and G2) in food and feed, a standard method involving a liquid extraction step followed by immunoaffinity purification and high-performance liquid chromatography (HPLC) is often used. In this work, this method is verified based on the requirements of ISO/IEC 17025 for the determination of aflatoxins in peanut kernel samples. All the method figures of merit including calibration, evaluation of limit of determinations (LODs) and limit of quantifications (LOQs), accuracy, precision, and uncertainty of the method are explained in detail. The accuracy of the applied method was verified by analysis of a CRM and calculation of the recovery. The relative standard deviations of the method (n = 6) were in the range of 4.99–7.85%. The LODs and LOQs of the method were found to be 0.15 and 0.50 μg. kg−1 for AFB1 and G1 and 0.06 and 0.2 μg kg−1 for AFB2 and G2, respectively. Finally, the uncertainties in the determination of aflatoxins concentrations, at the maximum permissible levels were calculated using the GUM procedure as 0.42, 0.094, 0.42, and 0.083 μg. kg−1 for AFB1, B2, G1, and G2, respectively. • Aflatoxins were quantified in peanuts by immunoaffinity column cleanup and HPLC-FLD. • Method verification was carried out based on ISO/IEC 17025 requirements. • Figure of merits of the method were calculated. • Uncertainties of the obtained results were calculated at maximum permissible level. [ABSTRACT FROM AUTHOR]

The aim of this study was to evaluate the promotive and/or inhibitory effects of NaCl, glucose, their combinations on biofilm formation and quorum sensing (QS) autoinducer-2 (AI-2) production on black tiger shrimp surfaces, using three strains of Vibrio parahaemolyticus . Initially, six different NaCl concentrations (0.5, 1, 2, 3, 4, and 5%) were evaluated for a maximum biofilm formation (∼6.3 log CFU/cm 2 ) at 30 °C. Inhibitory effects of glucose at six different levels (0.005, 0.01, 0.015, 0.02, 0.025, and 0.05%) were then investigated using the NaCl level previously found for a maximal biofilm formation. V. parahaemolyticus formed the best biofilm at 2% NaCl and the least biofilm at 5% NaCl, regardless of vibrio strain. In combination of 2% NaCl and glucose at different levels, the largest biofilm was observed at 0.015%, with the least biofilm seen at 0.05%, regardless of vibrio strain. Addition of salt and glucose more than the optimal level (2% salt and 0.015% glucose at 2% salt) inducted a stepwise inhibition of vibrio growth and biofilm formation in a continuous matter. In the visual evaluation, similar results were observed for vibrio growth, biofilm formation, live/dead cell detection, and quorum sensing. [ABSTRACT FROM AUTHOR]

This study evaluates the aflatoxin M1 (AFM1) contamination in 804 samples of raw milk from cow and buffalo, collected randomly in Campania and Calabria regions of Southern Italy over a two years period. The competitive enzyme linked immunosorbent assay (ELISA) method was used to analyze AFM1 in the samples. AFM1 levels result above the CCβ value of 0.004 μg/kg in 51 (12.3%) cow milk samples and in 28 (7.2%) buffalo milk samples. Positive results from screening analysis were confirmed by high performance liquid chromatography with fluorimetric detection (HPLC-FLD) after a procedure of centrifugation, extraction and immunoaffinity column clean-up of milk. Only one cow milk sample exceeded the maximum limit (0.05 μg/kg) set by the European Regulation. The occurrence of AFM1 contamination was significantly (p < 0.05) higher in cold season, particularly fall, than in warm season, principally spring. Our results indicate that feedstuff used in the buffalo and cow farms were not highly contaminated with aflatoxins, determining a good quality of the analyzed milk. Therefore, the AFM1 contamination of the milk does not represent a serious public health problem in both regions in Southern Italy. [ABSTRACT FROM AUTHOR]

The aim of this work was to determine the level of contamination of different kinds of commercial smoked meat and fish products from Polish market with polycyclic aromatic hydrocarbons (PAHs) for which the limiting values are established in the Commission Regulation (EU) 2015/1125. These PAHs are benzo( a )pyrene (BaP) and the sum of the following four PAHs: benzo( a )pyrene, benzo( a )anthracene (BaA), benzo( b )fluoranthene (BbFA) and chrysene (Chr). The research materials were fish, meat and chicken products smoked by the industrial or traditional techniques. The research methods included process of saponification of the samples, extraction of the polycyclic aromatic hydrocarbons fraction, and then qualitative and quantitative determination of PAHs by high performance liquid chromatography with fluorescence detection method (HPLC-FLD). The highest BaP content and the sum of the four polycyclic aromatic hydrocarbons (4PAHs) (36.51 mg/kg and 73.01 mg/kg, respectively) were found in canned smoked sprats in oil and these values exceeded the maximum levels given in the Commission Regulation (EU) 2015/1125. The analyzed products smoked by traditional technique contained significantly more PAHs as compared to the products smoked by the industrial technique or produced with smoke flavourings. [ABSTRACT FROM AUTHOR]

Aflatoxin M 1 (AFM 1 ) was analysed in 102 samples of fresh cow milk marketed in Penang and 45 samples of human milk from Penang Maternity Hospital. AFM 1 determinations were carried out by HPLC using fluorescence detector (FLD) after sample clean-up with immunoaffinity columns. Aflatoxin M 1 was detected in 4(4%) out of 102 cow milk samples analysed (4.0% occurrence). However the positive results were below 0.5 μg kg −1 which set as the maximum limit for AFM 1 in milk by Malaysian food regulations. None of the human milk samples were positive for AFM 1 contamination. [ABSTRACT FROM AUTHOR]

The consumption of agri-foods contaminated with mycotoxins poses a serious threat to human health. In this study, we evaluated the presence of total aflatoxins (AFs) and ochratoxin A (OTA) in various agri-food products of national and imported origin in Chile that are consumed daily. A total of 653 samples of cocoa (22), oats (50), ginger (62), pepper (131), coffee (42), raisins (34), turmeric (60), nutmeg (30), cereals (60), flour (47), walnuts (16), dried fruits (18), pistachios (10), hazelnuts (7), almonds (20), peanuts (35), and tea (9) were collected from 2018 to 2020 in markets and supermarkets in Chile by the Mycotoxin Monitoring Program of the Ministry of Health of Chile. Contamination by AFs occurred mainly in nutmeg, pepper, and ginger in 2018, as these compounds were not detected in 2020. The detection frequency for OTA was higher than that of the AFs, and it was mainly present in turmeric, ginger, and pepper. The Estimated Daily Intake (EDI) in nutmeg for AFs and OTA does not exceed the tolerable weekly or daily intake levels proposed by international bodies. [ABSTRACT FROM AUTHOR]

In this study, 50 dried eggplant and 50 dried green bell pepper samples were analyzed in terms of their aflatoxin and ochratoxin A (OTA) content. Aflatoxins G 2 , G 1 , B 2 , and B 1 , and OTA contents were analyzed using high-performance liquid chromatography with a flame ionization detector (HPLC–FID). Total aflatoxin and, as well as aflatoxin G 2 , G 1 , B 2 , and B 1 content in dried eggplant samples were ranged between 0.82 and 2.58, 0.10–0.23, 0.32–1.35, 0.12–0.67, and 0.17–0.71 μg kg −1 , respectively. Total aflatoxin and, as well as aflatoxin G 2 , G 1 , B 2 and B 1 content in dried green bell pepper samples were 0.81–2.42, 0.11–0.22, 0.32–1.38, 0.13–0.66, and 0.18–0.91 μg kg −1 , respectively. OTA content was varied from 8.88 to 21.35 μg kg −1 in eggplant samples, and from 15.38 to 24.70 μg kg −1 in dried green bell pepper samples. Of the dried eggplant samples and dried green bell pepper samples, 36% and 24% of them, respectively, had aflatoxin B 1 values which were below the minimum limit of detection (LOD) of 0.05 μg kg −1 . None of the analyzed samples exceeded the legal limit values of 10 μg kg −1 for total aflatoxin content, and 5 μg kg −1 for aflatoxin B 1 content. However, 80% of the dried eggplant samples and 100% of the dried green bell pepper samples exceeded the legal limit value for OTA content (15 μg kg −1 ). According to the results, it was concluded that dried vegetables should be examined in terms of their aflatoxins. It is essential to analyze OTA content more thoroughly, as it has the potential to pose a risk for public health, as well as for the economy. [ABSTRACT FROM AUTHOR]

Ochratoxin A (OTA), one mycotoxin produced by certain filamentous species of Aspergillus and Penicillium , is not known whether existing in Chinese liquors. However, specific method to detect OTA as well as OTA occurrence in Chinese liquors has not been reported so far. For this purpose, based on reversed phase/strong anion-exchange mixed-mode column (ProElut™ PXA), a novel solid-phase extraction (SPE) clean-up method followed by high-performance liquid chromatographic (HPLC) quantification was developed to detect OTA in Chinese liquors. Meanwhile, the matrix effects were evaluated by using the post-extraction spiked method with the signal suppression/enhancement (SSE) as the evaluation index. Under the optimized conditions, no matrix effects were found due to the SSE values below 20%, and the external standard method can be used to determine OTA in Chinese liquors. The recovery rate of spiked samples ranged from 81.6 to 100.8%. Intra-day and inter-day relative standard deviation were below 7.3% and 12.8%, respectively. The limits of detection and quantification were 0.006 and 0.02 μg/L, respectively. This approach was then applied to analyze the 76 samples from different geographical regions in China, including 40 strong aroma-, 30 light aroma- and 6 soy sauce aroma-type raw liquors. The results showed that OTA was detected in 9 samples with a maximum concentration of 0.17 μg/L. Considering that ∼12% of the samples were OTA positive, it is necessary to recommend a routine monitoring of this commodity. [ABSTRACT FROM AUTHOR]

An investigation on the occurrence of ochratoxin A (OTA) in baby food products consumed in Syria was conducted. A total of 42 samples of baby food formulae, including 30 cereal-based baby food and 12 fruit-based baby food formulae were analyzed using immunoaffinity columns (IAC) for sample clean-up and high performance liquid chromatography with fluorescence detection (HPLC-FD). According to the results in the present study, the mean recoveries of OTA from spiked cereal-based baby food and fruit-based baby food samples were in the range of 92.85–107.4% and 83.3–87.86%, respectively. While the limit of detection (LOD) and limit of quantification (LOQ) for OTA were 0.038 and 0.11 µg/kg for cereal-based baby foods and 0.05 and 0.17 µg/kg for fruit-based baby foods, respectively. Analytical results showed that 40.48% of the analyzed samples were found contaminated with OTA. Among the OTA contaminated samples, 43.33% samples of cereal-based baby food, and 33.33% samples of fruit-based baby food contained mean values of 0.094 and 0.093 µg/kg of OTA, respectively. Our findings show that contamination levels of OTA in all samples were lower than the permitted level set by European Commission Regulation. [ABSTRACT FROM AUTHOR]

This study describes the occurrence of polycyclic aromatic hydrocarbons (PAHs) in traditional yerba maté hot and cold infusions ( mate and tereré ), by monitoring the content of benz[a]anthracene, chrysene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[ah]anthracene, benzo[ghi]perylene and indeno[1,2,3-cd]pyrene (PAH8), that have been chosen as indicators for the occurrence and toxicity of PAHs in food by the European Food Safety Agency. PAH8 content in mate and tereré was determined by high performance liquid chromatography using fluorescence detection (HPLC-FLD). PAH8 contents in hot and cold maté infusions ranged from 371.2 to 2438.8 ng/L and from 19.2 to 937.3 ng/L, respectively. Benzo[a]pyrene contents varied between 37.0 and 373.9 ng/L in hot yerba maté infusions and between 7.0 and 92.1 ng/L in cold yerba maté infusions. None of the samples analyzed exceeded the World Health Organization criteria for drinking water, since the maximum level allowed for benzo[a]pyrene is 700 ng/L. [ABSTRACT FROM AUTHOR]

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

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

This study was aimed at simplifying the conventional aflatoxin HPLC-FLD analysis procedure for determining aflatoxins B1, B2, G1, and G2 by utilizing the advantage of immunoaffinity column (IAC) and normal-phase chromatography. Normally, a derivatization procedure is needed to enhance the fluorescence signal of aflatoxin quenched by the reversed-phase solvent used as the HPLC mobile phase. However, the proposed mobile phase (toluene/ethyl acetate/methanol/formic acid, 90 mL/6 mL/2 mL/2 mL) considerably enhanced the fluorescence signal by eliminating the quenching effect. IAC is a fast and reproducible method for sample clean-up, but the miscibility of the eluate is low in the normal-phase solvent. The miscibility of the eluate in the normal-phase solvent was improved by replacing methanol with acetonitrile as the eluent, dehydrating water after IAC elution, and mixing with toluene before HPLC analysis. The results demonstrate that the time-consuming procedures, such as nitrogen evaporation and iodine-derivatization, in the sample preparation were no longer needed, which improved the recovery and repeatability. The LOQ can be as low as 2.0-0.5-1.0–0.5 ng of aflatoxin B1-B2-G1-G2 per gram of peanut. All linearities (R2) of the four types of aflatoxin were greater than 0.999. The inter-day recovery rates of aflatoxin B1, B2, G1, and G2 at LOQ were 109%, 115%, 113%, and 77%, and the corresponding standard deviations were 12%, 8%, 5%, and 14%, respectively. The performance of the proposed method in analyzing raw peanuts was better than that of the official method (HPLC-FLD combined with post-column iodine-derivatization) and can meet the US FDA's standard for examining human food. The shelf-life of the proposed mobile phase was prolonged to 2 weeks under room temperature, further saving the use of solvent. Each analysis needed less than 25 mL of organic solvent to complete. Furthermore, the method can determine AF concentration in raw peanuts contaminated with more than 4.00 ng/g of total aflatoxins (containing 2.00 ng/g of aflatoxin B1, 0.50 ng/g of aflatoxin B2, 1.00 ng/g of aflatoxin G1, and 0.50 ng/g of aflatoxin G2). • Fluorescence intensity was enhanced with normal phase HPLC system. • Limit of detection of the proposed method can be as low as that of post-column derivatization method. • The proposed method significantly reduced time and labor for sample preparation. • Less than 30 mL of solvent was consumed for each sample analysis. [ABSTRACT FROM AUTHOR]

This study aims to develop HPLC-FLD method and verify its applicability for Ethyl Carbamate (EC) determination in Chinese spirits, and to investigate the mechanism for EC generation and its influencing factors. HPLC-FLD with prior derivatization with 9-xanthydrol was used for the EC detection. Optimal reaction condition and the parameters usually tested in the method validation were identified and evaluated. Most appropriate mobile phase is sodium acetate solution with pH value at 7.2. Optimal alcohol strength and reaction time for derivatization are 38–42% and 50 min respectively. Good linearity was obtained with correlation coefficient greater than 0.9998; limit of detection and quantitation were 1.82 and 5.34 μg/L; recovery rate was 96.67% (±6.59%), and method precision was less than 5% (RSD). No significant difference was found in EC determination measured by HPLC-FLD and GC/MS (p > 0.05) indicating HPLC-FLD may be a suitable alternative to GC/MS with greater convenience and lower cost. The average EC content in the Chinese spirit was 39.3 μg/L (ND. to 79.1 μg/L, n = 90), and EC was mainly produced during storage. Raw material profile, brewing time, and storage time and temperature were suggested as main factors influencing EC content; moreover, lowering the storage temperature can effectively reduce EC production. Hydrocyanic acid was concluded as the EC precursor in Chinese spirits. A preliminary multiple regression model based on the storage temperature and time was produced to forecast the EC content in Chinese spirits, and this could be further developed in future research including more influencing factors. [ABSTRACT FROM AUTHOR]

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

The immunoaffinity column cleanup method coupled with HPLC separation and fluorescence detection is still one of the most frequently used quantitative methods for routine analyses of AFM1. In this study, aflatoxin M1 (AFM1) was quantified with a chromatography column packed with 2.6 μm core-shell particles on a conventional HPLC. A large volume of solvent (100 μL) was injected into the highly efficient column without any noticeable reduction in separation performance with the help of stepwise gradient elution. The instrumental conditions were optimized by response surface analysis methodology (RSM) with a three-level three-factor Box–Behnken design. The use of core-shell columns on conventional HPLC for AFM1 analysis under the optimized instrumental conditions leads to increased analytical performance compared with traditional totally porous columns without the heavy costs associated ultra-high-pressure instruments. Moreover, the improved instrumental sensitivity enables simplified sample preparation by avoiding any solvent replacement. The method could be easily applied to enhance the sensitivity of HPLC-FLD for AFM1 analysis that is based on isocratic elution and is more widely used. The method was successfully applied to 40 raw milk samples collected in summer from 20 cattle ranches located in two different provinces in southwestern China. [ABSTRACT FROM AUTHOR]

In this study, a total of 370 rice samples collected from six provinces in China were surveyed for the presence of aflatoxins (AFs) and ochratoxin A (OTA) using dispersive liquid–liquid microextraction coupled to liquid chromatography with fluorescence detection. The results obtained in this survey showed that 63.5% (235/370) and 4.9% (18/370) of rice samples contained detectable amounts of AFs and OTA, respectively. The average levels of AFB 1 , total AFs and OTA in positive samples were 0.60, 0.65 and 0.85 μg/kg, respectively. AFB 1 and AFB 2 were present in samples from all six provinces and could be quantified in 87 and 32 samples, respectively. OTA was present in samples from four provinces and could be quantified in 6 samples. The percentages of rice samples with AFB 1 and OTA levels above the EU limit were 1.4% (5/370) and 0.3% (1/370), respectively. The results show that the levels of the mycotoxins in rice are below regulatory limits and the rice commodities are generally safe. It also indicates the need to establish a continuous monitoring program to prevent and manage the occurrence of these contaminants. [ABSTRACT FROM AUTHOR]

Fumonisins (FBs) mainly produced by some Fusarium species, such as Fusarium verticillioides and Fusarium proliferatum , are worldwide occurring in maize. Fumonisin B 1 (FB 1 ) and Fumonisin B 2 (FB 2 ) are the most abundant and the most toxic among all the known fumonisins. The fumonisins contamination of maize has raised serious economics, food safety and human health problems. The aim of this study was to determine the incidence and contamination levels of fumonisins in maize from different areas in China. A total of 146 samples of maize were collected in 2012 after maize harvest from three provinces including Gansu, Sichuan and Guizhou in China and analyzed for FB 1 and FB 2 using high-performance liquid chromatography coupled with fluorescence detection following o -phthalaldehyde derivatization. The results showed that the incidence and mean levels of fumonisins (FB 1 + FB 2 ) contamination for all collected maize samples were 39.7% and 497 ng/g, respectively. Among the three provinces, the mean level of total fumonisins contamination of maize samples from Guizhou province was 754 ng/g, which was higher than that of Sichuan (527 ng/g) and Gansu (202 ng/g). 3.4% of all maize samples had total fumonisins levels higher than 2000 ng/g set by the Food and Drug Administration of the United States and 1.4% had the levels in excess of 4000 ng/g recommended by the European Commission. The possible level of fumonisins exposure for the consumers (0.08 μg/kg of body weight per day) is within the provisional maximum tolerable daily intake of 2.0 μg/kg of body weight per day set up by the Joint FAO/WHO Expert Committee on Food Additives (JECFA). Nevertheless, more efforts should be made to prevent and control fumonisins contamination of maize and to minimize the potential risk to health of the consumers. [ABSTRACT FROM AUTHOR]

Abstract: A total of 144 breakfast cereal and snack samples collected from six areas in the United States (U.S.) were surveyed for the presence of ochratoxin A (OTA). All samples are the processed products including mainly corn, oat, wheat, and rice. The analytical methods in this study were immunoaffinity columns (IAC) and high performance liquid chromatography (HPLC) with fluorescence detection (FLD). The method provided recoveries of OTA from all sample matrices in the range of 95–100%. The limits of detection and limits of quantification for OTA were 0.032 and 0.10 ng/g for corn, wheat, and rice based samples; 0.038 and 0.12 ng/g for oat based samples, respectively. Analytical results showed that 75 samples (52%) were contaminated with OTA in the range of 0.10 and 7.43 ng/g. Among the OTA contaminated samples, 40% were labeled as organic and 60% were conventional with mean concentrations of 1.21 and 1.07 ng/g, respectively. There were ten contaminated samples, all from oat based products, exceeding the maximum limits for OTA by European Commission Regulation (3 ng/g) in cereal based products. [Copyright &y& Elsevier]

Abstract: In this study, a sensitive high performance liquid chromatography coupled to a fluorescence detector (HPLC-FLD) method after post-column derivatisation was applied for the presence of aflatoxins (AFs) in 151 pistachios and 151 groundnuts from Turkey. Samples were collected between January 2010 and December 2012 in two provinces of Turkey and checked for AFs levels. Quantification limits were 0.11, 0.11, 0.12 and 0.14 μg kg−1 for aflatoxin B1 (AFB1), aflatoxin B2 (AFB2), aflatoxin G1 (AFG1) and aflatoxin G2 (AFG2), respectively. AFs were present in 14.6% of pistachios (22/151) and 19.2% of groundnuts (29/151) at total AFs levels ranging from 0.26 to 385 μg kg−1 and from 0.16 to 60.9 μg kg−1, respectively. Seven pistachio samples were above the European maximum tolerable limit (MTL) of 8 μg kg−1 for AFB1, while total AFs concentration exceeded the MTL of 10 μg kg−1 in eight pistachio samples. For groundnuts, eight and six samples exceeded MTL of 2 and 4 μg kg−1 for AFB1 and total AFs, respectively. [Copyright &y& Elsevier]

Abstract: A facile and inexpensive method using solid phase extraction (SPE) on OASIS HLB and HPLC with fluorescence detector (FLD) determination of aflatoxin M1 (AFM1) in liquid milk and milk powder was described. The detection limits of this method provided were 0.006 μg/kg for liquid milk and 0.026 μg/kg for milk powder. The recoveries obtained in all food matrices were between 85.4 and 96.9%, and the RSDs were between 0.8 and 3.6%. Furthermore, a total of 31 samples were detected using OASIS HLB and immunoaffinity column (IAC) as a comparison, both cleanup methods obtained consistent results. The level of AFM1 contamination found in 8 samples among the tested samples did not exceed the Chinese legal limit (0.5 μg/kg). This method was applied successfully to analyse AFM1 in liquid milk and milk powder without interference peaks. [Copyright &y& Elsevier]

Abstract: The chromatographic HPLC-FLD method was introduced for the first time to identify and quantitatively determine individual Paralytic Shellfish Poisoning toxins accumulated in aquacultured shellfish from Croatian coastal waters. Populations of Mediterranean mussels (Mytilus galloprovincialis) were contaminated with PSP toxins throughout January to April 2009 leading to the positive test results by Mouse Bioassay (MBA). Until 2009 there was no evidence of PSP toxins in the examined samples. For the first time an instrumental method revealed the PSP toxin profile of samples taken along the eastern Adriatic coast and identified saxitoxin (STX) as the main representative of this toxin group that may cause paralysis and death in consumers of contaminated shellfish. This phenomenon may have serious health and economic consequences. Following these potential consequences, marine biotoxins (PSP, ASP and DSP) are continuously assessed in bivalves from 25 breeding and harvesting areas along the Croatian Adriatic coast. Positive MBA results were confirmed by instrumental method in two out of three recorded samples. Saxitoxin was the dominant PSP toxin extracted from contaminated mussels within the range of 53.17–1298.17 μg g−1, that contributed more than 70% to the total shellfish toxicity, followed by gonyautoxins 2 and 3 (GTX 2,3) which contributed 27% and decarbamoylsaxitoxin (dcSTX) that accounted for less than 2%, considering all stations. [Copyright &y& Elsevier]

Abstract: Ochratoxin A (OTA) is a mycotoxin that can be found in several food commodities including cereals, wine, coffee, cacao, spices or dried fruits, resulting in chronic human exposure. The aim of our study was to investigate the presence of OTA in widely consumed cereal-derived products commercialized in Turkey. A total of 142 samples were collected from different supermarkets and traditional bazaars in Istanbul during 2008–2010 years. The analytical methods used in our study involved the liquid/liquid extraction of OTA, immunoaffinity clean-up and high performance liquid chromatography determination with fluorescence detection. The frequencies of OTA contamination were 21.62%, 19.05% and 55.95% and the mean concentrations of positive samples were 0.32 μg/kg, 0.14 μg/kg, 0.41 μg/kg for breakfast cereals, cereal-based baby foods and tarhana samples, respectively. Our findings show that contamination levels of OTA in all cereal-derived products were lower than the permitted level by European Commission Regulation. [Copyright &y& Elsevier]

Abstract: A new method for the determination and analysis of aflatoxins in noodles, based on the use of the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) procedure, enhanced with a high performance liquid chromatography–coupled to a fluorescence detector (HPLC–FLD) has been developed. The method excludes the use of dispersive solid-phase extraction (dSPE) extraction cleanup step to reduce time and cost of analysis. Separation of the four(4) aflatoxins with higher selectivity and sensitivity, and within reasonable limits of retention time, was performed by using an isocratic mobile phase of water/methanol/acetonitrile (65/25/10) at a column temperature of 30 °C. Optimization of sample preparation and analytical conditions gave recoveries in the range of 75%–107% at spike levels of 5.0–20.0 μg/kg, and relative standard deviations (RSDs) lower than 13% in all the cases. The repeatability and reproducibility results were in range of 2.0–12.3% and 3.4–16.5% respectively. Additionally, the limits of detection (LOD) (0.01–1.00 μg/kg) and the limits of quantification (LOQ) (0.05–1.80 μg/kg) of these aflatoxins are well within the legal limits set by the European Union (EU). [Copyright &y& Elsevier]

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

Abstract: An analytical method based on HPLC-FLD with prior derivatization with 9-xanthydrol for the determination of ethyl carbamate (EC) in cider spirits is reported. The parameters usually examined in the method validation were evaluated. Good linearity was obtained with a correlation coefficient exceeding 0.9999, the limits of detection and quantitation being 1.64 and 3.56μg/L, respectively. Recoveries ranged between 94% and 98%, while the precision of the method was <5% (RSD). The method was used to determine EC in samples from different origins with the aim of completing the characterization of cider spirits. Values obtained were usual for this type of drink, ranging between the lower limit of quantitation and 67μg/L. [Copyright &y& Elsevier]

Coffee is today one of the most popular beverages in the world and the determination of its authenticity is an important issue considering the increase of adulteration cases in the last years. In this work, a simple and efficient non-targeted HPLC-FLD fingerprinting method was employed to detect and quantify adulteration levels in coffee samples by partial least squares (PLS) regression to guarantee food integrity and authenticity. For that purpose, different adulteration cases, involving both coffee production region and variety, were evaluated by pairs (Colombia-Ethiopia, Colombia-Nicaragua, India-Indonesia, Vietnam Arabica-Vietnam Robusta, Vietnam Arabica-Cambodia, and Vietnam Robusta-Cambodia adulteration cases). Overall, the proposed non-targeted HPLC-FLD fingerprinting strategy showed very good results with PLS cross-validation and prediction errors below 3.4% and 7.5%, respectively, for adulteration levels below 15%. Therefore, non-targeted HPLC-FLD fingerprints demonstrated to be suitable to assess coffee integrity and authenticity in the control and prevention of frauds. • Chromatographic fingerprints and chemometrics for coffee authentication. • Detection of coffee frauds according to production region and coffee specie. • PLS quantitation of adulterated coffees down to 15% adulteration levels. • PLS prediction errors below to 7.5% were reached. [ABSTRACT FROM AUTHOR]

Economically motivated food fraud has increased in recent years, with adulterations and substitutions of high-quality products being common practice. Moreover, this issue can affect food safety and pose a risk to human health by causing allergies through nut product adulterations. Therefore, in this study, high-performance liquid chromatography with fluorescence detection (HPLC-FLD) fingerprints were used for classification of ten types of nuts, using partial least squares regression-discriminant analysis (PLS-DA), as well as for the detection and quantitation of almond-based product (almond flour and almond custard cream) adulterations with hazelnut and peanut, using partial least squares regression (PLS). A satisfactory global nut classification was achieved with PLS-DA. Paired PLS-DA models of almonds in front of their adulterants were also evaluated, producing a classification rate of 100%. Moreover, PLS regression produced low prediction errors (below 6.1%) for the studied adulterant levels, with no significant matrix effect observed. • Chromatographic fingerprints and chemometrics for nut authentication and safety. • Good classification of nuts according to their type by HPLC-FLD fingerprinting. • PLS quantitation of almond-based products adulteration with hazelnut and peanut. • Prediction errors down to 6.1% were reached. [ABSTRACT FROM AUTHOR]

This study analyzed 15 polycyclic aromatic hydrocarbons (PAHs) in 170 youtiao (Chinese dough sticks) samples collected from Shandong Province of China, which were determined using high performance liquid chromatography-fluorescence detection (HPLC-FLD). The results indicated that the incidence rate of PAHs compounds was 89.4% and the mean concentration of 15 PAHs was 65.8 μg/kg. Naphthalene (Nap) was detected with the highest concentration and the largest incidence rate. One sample exceeded the maximum level of 1 μg/kg for the carcinogenic benzo(a)pyrene (BaP) in cereals and cereal-based products set by European Union (EU), while 47 samples exceeded the maximum level of 1 μg/kg for PAH4 set by EU. The dietary exposure of PAHs and the potential human health risk assessment were assessed using estimated daily intake (EDI), target hazard quotient (THQ), and the incremental lifetime cancer risk (ILCR). EDI values were below the intake range reviewed by the European Food Safety Authority (EFSA) for each class of contaminant. The THQ values were below the safe standard of 1, thus the risk to develop chronic systemic effects due to individual PAH was low. The ILCR results for children, adolescents, adults, and seniors were all lower than the priority level (1 × 10−4), implying no significant cancer risk related to youtiao consumption for local population. Further data are still needed for proper management of the risks associated with PAHs in youtiao samples. • Polycyclic aromatic hydrocarbons (PAHs) contamination in 170 youtiao was studied. • The 15 PAHs levels in youtiao were analyzed and compared with published studies. • The raw materials and technological impact on PAH contamination were discussed. • The dietary exposure associated with the consumption of youtiao was estimated. [ABSTRACT FROM AUTHOR]