Determination of Phthalates into Vegetable Oils by Isotopic Dilution Gas Chromatography Mass Spectrometry

The presented method for the determination of a number of phthalic acid esters into oily media is based on their extraction by acetonitrile with precipitation under freezing and subsequent solid-phase extraction using alumina. This technique was checked as the best procedure to separate lipophilic phthalates from fatty media achieving elimination of contamination by excess use of solvents. Extracted phthalates are determined in acetonitrile solutions with gas chromatography in conjunction to isotopic dilution mass spectrometry using D4 isotopic labeled derivatives. Full validation of the method was carried out and background effect was examined. Method calibration for extraction from oil resulted in limit of detection (LOD) of 7–10 ng g^?1 and limit of quantification (LOQ) of 20–50 ng g^?1 for DMP, DEP, DiBP, DBP, DEHP, and BBP and in LOD 500 ng g^?1 and LOQ of 1,500 ng g^?1 for DiNP and DiDP. Real samples of virgin olive oil from olive press establishments from three different areas were analyzed and the phthalates content was below detection limit for all phthalic esters under consideration for nonindustrial areas and in measurable concentrations for industrial areas specifically with regard to DiBP.     

Bisphenol A in domestic and imported canned foods in Japan

Bisphenol A (BPA) concentrations were surveyed in 100 domestic and 60 imported canned foods purchased from the Japanese market in 2011–12. BPA was extracted from the canned foods, derivatised by ethylation and analysed using GC-MS. In the domestic canned foods, the maximum and average BPA concentrations were 30 and 3.4 ng g^?1, respectively, while in the imported canned foods they were 390 and 57 ng g^?1, respectively. The BPA level in the domestic canned foods was significantly lower than that in the imported canned foods. Based on these results, the intakes of BPA from the domestic and imported canned foods in Japan were estimated as 644 ng person^?1 day^?1. The Japanese BPA intake was the second lowest following New Zealand, although imported canned foods increased. It was sufficiently lower than the tolerable daily intake of EFSA and the USEPA. The drastic reduction of BPA in the domestic canned foods should be due to the ‘BPA reduced cans’ that Japanese can manufacturers had developed in the late 1990s and became widely used in Japan.     

A survey of bisphenol A and other bisphenol analogues in foodstuffs from nine cities in China

Bisphenol A (BPA) is a high-production-volume chemical that is widely used in polycarbonate plastics and epoxy food-can coatings. Following several studies that have reported adverse effects of BPA over the past decade, other bisphenol analogues, such as bisphenol F (BPF), bisphenol S (BPS), bisphenol AF (BPAF), and bisphenol B (BPB), have been gradually developed as substitutes for BPA in several applications. Nevertheless, few studies have reported on the occurrence of compounds other than BPA in foodstuffs. In this study, 289 food samples (13 categories: cereals and cereal products, meat and meat products, fish and seafood, eggs, milk and milk products, bean products, fruits, vegetables, cookies/snacks, beverages, cooking oils, condiments, and others), collected from nine cities in China, were analysed for eight bisphenol analogues using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). BPA and BPF were found widely in foodstuffs at concentrations ranging from below the limit of quantitation (LOQ) to 299 ng g^–1 (mean = 4.94 ng g^–1) and from below the LOQ to 623 ng g^–1 (mean = 2.50 ng g^–1), fresh weight, respectively. The highest total concentrations of bisphenols (∑BPs: sum of eight bisphenols) were found in the category of vegetables that included canned products (mean = 27.0 ng g^–1), followed by fish and seafood (16.5 ng g^–1) and beverages (15.6 ng g^–1). ∑BP concentrations (mean = 2–3 ng g^–1) in milk and milk products, cooking oils, and eggs were low. Food samples sold in metallic cans contained higher mean ∑BP concentrations (56.9 ng g^–1) in comparison with those packaged in glass (0.43 ng g^–1), paper (11.9 ng g^–1), or plastic (6.40 ng g^–1). The daily dietary intakes of bisphenols were estimated, based on the mean concentrations measured and daily consumption rates of foods, to be 646 and 664 ng kg^–1 bw day^–1 for men and women, respectively.     

Simultaneous Determination of Seven Polycyclic Aromatic Hydrocarbons in Coffee Samples Using Effective Microwave-Assisted Extraction and Microextraction Method Followed by Gas Chromatography-Mass Spectrometry and Method Optimization Using Central Composite Design

In this research, for the first attempt, we successfully determined seven polycyclic aromatic hydrocarbons (PAHs) in various coffee samples using microwave-assisted extraction and dispersive liquid-liquid microextraction (MAE-DLLME) coupled with gas chromatography-mass spectrometry (GC-MS). The effects of most important variables in microextraction step were investigated and optimized using response surface methodology (RSM) based on central composite design. The calibration curves were linear in the range of 1–200 ng g^?1, with a correlation coefficient (R ²) higher than 0.989. Limits of detection were obtained between 0.1 and 0.3 ng g^?1. The relative standard deviations (RSD%) for seven repeated analysis were less than 8% for all PAH compounds at a concentration of 10 ng g^?1. Relative recoveries were obtained 88.1–101.3%. The satisfactory results obtained by the proposed method and the comparison of these results with previous methods demonstrated that the MAE-DLLME-GC-MS is an accurate, rapid, and reliable sample-pretreatment method with low consumption of the organic solvent.     

Headspace solid-phase microextraction coupled to gas chromatography-tandem mass spectrometry for the determination of haloanisoles in sparkling (cava and cider) and non-sparkling (wine) alcoholic beverages

A highly sensitive analytical method was developed to determine 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and 2,3,4,5,6-pentachloroanisole (PCA) in sparkling alcoholic beverages. The method was based on the use of headspace solid-phase microextraction (HS-SPME) using a polydimethylsiloxane (PDMS) fibre. It was coupled to gas chromatography-triple quadrupole tandem mass spectrometry (GC-QqQ-MS/MS) for the detection and quantification of the target haloanisoles. The method was fully automated and no sample preparation was needed. The method was validated for alcoholic beverages. The influence of CO₂ on the extraction efficiency was also evaluated for the studied sparkling drinks (cava and cider). All the calibration curves showed good linearity (R² > 0.98) within the tested range (1–50 ng l^?1). Recoveries were evaluated at three different levels (1, 5 and 50 ng l^?1) and were always between 71% and 119%. Precision was expressed as relative standard deviation (RSD), and was evaluated as intra- and inter-day precisions, with values ≤ 22% in both cases. Limits of quantitation (LOQs) were ≤ 0.91 ng l^?1, which are below the sensory threshold levels for such compounds in humans. The validated method was applied to commercial samples, 10 cavas and 10 ciders, but it was also used for the analysis of nine red wines and four white wines, demonstrating the further applicability of the proposed method to non-sparkling beverages. TCA was detected in most samples at up to 0.45 ng l^?1.     

Determination of biogenic amines in selected Malaysian food

The biogenic amines tryptamine (TRP), putrescine (PUT), histamine (HIS), tyramine (TYR) and spermidine (SPD) were determined in 62 selected food items commonly consumed in Malaysia. This include the local appetisers “budu” and “cincalok”, canned fish, salt-cured fish, meat products, fruit juice, canned vegetables/fruits and soy bean products. After the aqueous extraction, the samples were derivatised with dansyl chloride before analysing using reversed phase HPLC with UV detection. Mean levels of TRP, PUT, HIS, TYR and SPD in eight budu samples were 82.7, 38.1, 187.7, 174.7 and 5.1 mg kg⁻¹, respectively. The main biogenic amines found in cincalok were PUT, HIS and TYR where the mean values were 330.7, 126.1 and 448.8 mg kg⁻¹, respectively. With the exception of “pekasam” and “belacan”, significantly lower levels of biogenic amines were found in canned fish and salt-cured fish samples. Non detectable or low levels of biogenic amines were found in meat, fruit juice and canned vegetables/fruit samples.     

Furan in commercial baby foods from the Spanish market: estimation of daily intake and risk assessment

ABSTRACT

The occurrence of furan in commercial baby food samples from the Spanish market was evaluated using an automated headspace solid-phase microextraction method coupled to gas chromatography-mass spectrometry (HS-SPME-GC-MS). A total of 76 baby food samples including infant formula, baby cereals, fruit in cans and/or jars, vegetables, meat, and fish, were surveyed for furan content. The lowest concentration of this compound was found in infant formula (<0.02–0.33 ng ml^?1), and cereal-based food (0.15–2.1 ng g^?1) while baby food containing fish showed the highest concentrations (19–84 ng g^?1). Following recommendation of the European Food Safety Authority (EFSA), the effect on furan content was evaluated of consumer home preparation of foods, heating and handling. Furan concentrations were reduced by up to 35% when samples were heated in a dish using microwave oven and by up to 53% when a hot water bath was used. Finally, we estimated the furan intake from baby food consumption (0.002–1.18 µg kg^?1 body weight day^?1) and we calculated the margin of exposure (MOE) from samples as purchased and also after home preparation of the food. For infant formula and cereal baby foods, the MOEs (26,278–412,776) indicated no infant health concern or priority, while for meat and fish-based baby foods the values pointed to a potential public health risk, even considering the furan losses during preparation at home.     

Occurrence of 13 volatile organic compounds in foods from the Canadian total diet study

Volatile organic compounds (VOCs) are ubiquitous in the environment due to evaporation and incomplete combustion of fuels, use of consumer and personal care products, etc. and they can accumulate in foods. Some VOCs in foods can also be formed during food processing and preparation and migrate from food packaging. In this pilot study, a GC-MS method based on headspace solid-phase microextraction (SPME) was validated and used to analyse selected individual foods which can be consumed directly and 153 different total diet composite food samples for 13 VOCs. Vinyl chloride was not detected in any of the 153 composite food samples, while the other 12 VOCs were detected at various frequencies, with m-xylene being the most frequently detected (in 151 of the 153 samples), followed by toluene (145), 1,3,5-trimethylbenzene (140), ethylbenzene (139), styrene (133), 1,2,4-trimethylbenzene (122), benzene (96), p-dichlorobenzene (95), n-butylbenzene (55), chloroform (45), naphthalene (45) and trichloroethylene (31). Concentrations of the 12 VOCs in most of the food composite samples were low, with the 90th percentiles from 1.6 ng g^–1 for n-butylbenzene to 20 ng g^–1 for toluene. However, some VOCs were detected at higher levels with maxima, for example, of 948 ng g^–1 for m-xylene and 320 ng g^–1 for ethylbenzene in chewing gum, 207 ng g^–1 for styrene and 157 ng g^–1 for toluene in herbs and spices. VOCs were detected at higher levels in most of the individual food items than their corresponding composite samples, for example, the average chloroform concentration in the individual canned soft drinks was 20 ng g^–1 compared with 3.0 ng g^–1 in their composite, and the average toluene concentration in the individual canned citrus juice was 96 ng g^–1 compared with 0.68 ng g^–1 in their composite. Thus, for determination of VOCs in foods which can be consumed directly, their individual food items should be analysed whenever possible for accurate exposure assessment.     

Optimization of Headspace Single-Drop Microextraction Coupled with Gas Chromatography–Mass Spectrometry for Determining Volatile Oxidation Compounds in Mayonnaise by Response Surface Methodology

In this assay, headspace single-drop microextraction (HS-SDME) coupled with gas chromatography–mass spectrometry (GC–MS) as a simple, low-cost and rapid method has been developed and validated for determining volatile oxidation compounds including hexanal and heptanal in mayonnaise. The main microextraction variables affecting the HS-SDME procedure such as extraction temperature and time, stirring rate, and amount of NaCl were optimized by response surface methodology employing a central composite design. Obtained results demonstrated that higher yield of extracted analytes could be achieved under the following optimal conditions: extraction temperature of 45 °C, extraction time of 16 min, stirring rate at 700 rpm, and addition of 2 g NaCl. The optimized HS-SDME/GC–MS method was validated for oxidized mayonnaise samples (50 °C/48 h) by calculating analytical parameters (linearity, precision, accuracy, and sensitivity). Good linearity (R ²?>?0.99) was observed by plotting calibration curves of extracted hexanal and heptanal over the concentration range of 0.025–10 μg g^?1, and the repeatability of the method, expressed as relative standard deviation, were found to be 4.04 % for hexanal and 3.68 % for heptanal (n?=?7). After the microextraction process of spiked mayonnaise sample, high levels of relative recovery were obtained for hexanal (107.33 %) and heptanal (91.43 %). The detection limits were 0.008 ng g^?1 and 0.021 ng g^?1 for hexanal and heptanal, respectively, while quantification limits of hexanal and heptanal were calculated to be 0.027 ng g^?1 and 0.071 ng g^?1, respectively. The possibility of the HS-SDME followed GC–MS to determine and quantify volatile oxidation compounds such as hexanal and heptanal was confirmed by analyzing commercial fresh mayonnaise stored at 4 and 25 °C during 3 months.     

Quantification of aristolochic acids I and II in herbal dietary supplements by ultra-high-performance liquid chromatography–multistage fragmentation mass spectrometry

A rapid, selective and sensitive ultra-high-performance liquid chromatography–multistage fragmentation mass spectrometry (UHPLC-MS³) method was developed and evaluated for the determination of aristolochic acids I and II (AA I and II) in herbal dietary supplements. A hybrid triple quadrupole/linear ion-trap mass spectrometry was used to monitor MS³ ion transitions m/z 359.2 > 298.1 > 268.0 and m/z 329.2 > 268.2 > 238.0 to detect AA I and II, respectively. The extraction and clean-up of target analytes from dry powdered samples was performed using the quick, easy, cheap, effective, rugged and safe (QuEChERS) procedure. Herbal liquid extracts were analysed directly. Average recoveries ranged from 89% to 112%, with relative standard deviations (RSDs) ranging from 3% to 16%. Limits of quantification (LOQs) estimated for three selected matrices were as follows (AA I/II): 5/10 ng g^?1 (tablets); 25/50 ng g^?1 (capsules); and 2.5/5.0 ng ml^?l (liquid herbal extract). The method was applied in a limited survey of 30 herbal products marketed in the United States via the Internet. AA I and II were detected in 20% and 7%, respectively, of tested samples.     

Are Chileans exposed to dietary furan?

Chilean consumer preferences include foods that may contain considerable amounts of furan, a potential human carcinogen. However, there is no information regarding dietary exposure to furan in Chile. Thus, the objective of this work was to determine the Chilean exposure to dietary furan. To accomplish this objective, the furan concentration of 14 types of commercial foods processed at high temperature were analysed based on a modified headspace-GC/MS (HS-GC/MS) method in which the limits of detection for different food matrices ranged from 0.01 to 0.6 ng g^?1. In addition, a risk assessment was made with exposure estimates based on dietary data from national studies on different age groups (9-month-old babies, school children, adults and elderly people). Of the food items surveyed “American”-type coffee (espresso coffee plus hot water) obtained from automatic coffee machine (936 ng g^?1) and low moisture starchy products like crisps and “soda”-type crackers showed the highest furan concentrations (259 and 91 ng g^?1, respectively). Furthermore, furan was also found in samples of breakfast cereals (approximately 20 ng g^?1), jarred fruit baby foods (8.5 ng g^?1) and orange juice (7.0 ng g^?1). School children (aged 9–13 years) represented the highest intake of furan (about 500 ng kg^?1_bw day^?1), with margins of exposure of 2479 and 2411, respectively, which points to a possible public health risk.     

Levels and distribution of PBDEs and PFASs in pork from different European countries

ABSTRACT

Meat and meat products are included in a great number of human diets. However, the great consumption of meat needs to be controlled for the presence of traces of contaminants. The European Commission has not stated maximum limits for some environmental pollutants such as the perfluoroalkyl substances (PFASs) and polybrominated diphenyl ether (PBDE); the European Food Safety Authority (EFSA) Scientific Panel has recommended that more occurrence data for PFASs in food should be collected to improve the accuracy of future exposure calculations. Therefore, the distribution of PFASs and PBDEs trace contaminants from eight EU Member States were investigated through liquid chromatography coupled to high-resolution mass spectrometry (LC-HRMS) and Gas Chromatography-Mass Spectrometry (GC-MS/MS). No PFASs were detected, except perfluorooctanoic acid, in only one Austrian sample at the concentration of 0.531 ng g^?1. PBDEs were detected in 3 out of 77 samples: one from Germany showed the presence of all congeners analysed in the concentration range 0.53–0.77 ng g^?1, the others, from Netherland and Italy, respectively contained PBDE 153 (0.53 ng g^?1) and PBDE 100 (0.62 ng g^?1). The results show that the analysed samples do not pose a risk for human beings in regard to PFASs and PBDEs. Further studies are needed to keep monitoring their presence in foodstuff, as it has been suggested by European Commission.     

Analysis and risk assessment of ethyl carbamate in various fermented foods

Ethyl carbamate (EC) was analyzed in fermented foods, comprising various matrices; subsequently, a risk assessment for EC was carried out. In total, 128 fermented foods were purchased from department stores and traditional markets in Korea. The samples comprised 55 lactic acid–fermented vegetable (kimchi), 53 fermented soybean paste (doenjang, gochujang, cheonggukjang, and ssamjang), 20 fermented fish products (jeotgal), 18 yoghurt, 37 bread, 12 cheese, and 23 vinegar samples. The level of EC in fermented soybean pastes ranged from not detectable to 240.2 ng g^?1. EC was not detected in kimchi, jeotgals, yoghurt, and cheese. Bread and vinegar contained EC up to 3.70 and 16.79 ng g^?1, respectively. The estimated daily intake and chronic daily intake of EC were 1.98 ng kg body weight (bw)^?1 day^?1, 1.50 ng kg bw^?1 day^?1, respectively. Excess cancer risk and margin of exposure of EC were 7.5 × 10^?8 and 151,515, respectively.     

Comparison of Two Analytical Methods for the Analysis of Methylmercury in Fish

In this study, we compared a high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry (HPLC-ICP-MS) method and an isotope dilution gas chromatography mass spectrometry (ID-GC-MS) method for the analysis of methylmercury (MeHg) in fish samples. Using HPLC-ICP-MS, the limit of detection (LOD) was 2.0 ngHg?·?g^?1 for inorganic Hg and was 5.0 ngHg?·?g^?1 for MeHg. In comparison, the LOD for MeHg was 3.4 ngHg?·?g^?1 for using ID-GC-MS. Certified reference material (CRM) results agreed well with certified values for both methods. The mean recovery for analysis of CRM BCR 463 by HPLC-ICP-MS was 99?±?2.1 % for MeHg and was 103?±?2.1 % for total Hg. Two CRMs, BCR 463 and CRM DORM2, were analyzed by ID-GC-MS, the mean recovery of MeHg was 87?±?1.9 % for BCR 463, and the mean recovery of MeHg was 102?±?2.9 % for CRM DORM2. Matrix samples spiked with Hg or MeHg at various concentrations were analyzed by two methods. For HPLC-ICP-MS method, the mean recovery for MeHg spiked samples was 93?±?4.2 %. For ID-GC-MS method, the mean recovery for MeHg spiked samples was 91?±?5.2 %. A total of 19 predatory fish and 54 tuna fish samples were analyzed using both methods. No significant difference was observed between the MeHg data generated from both methods. The average relative standard deviation (RSD) between the two datasets for 19 predatory fish samples was 8.8 %. The average RSD between two datasets for 54 tuna fish samples was 4.4 %.The HPLC-ICP-MS method offers substantial advantages over the method of ID-GC-MS because the former method can determine the total mercury (Hg) and MeHg in a single chromatographic run and the analysis time is much shorter. The latter method is time consuming due to overnight digestion and having to conduct presample analysis for signal-matched isotope dilution spiking and requires more expensive isotope labeled reagents.     

Influence of food condiments on the formation of carcinogenic heterocyclic amines in cooked chicken and determination by LC-MS/MS

Heterocyclic amines (HCAs) are known to be suspected human carcinogens produced by high-temperature cooking of protein-rich foods such as meat and fish. In the present study, the influence of numerous food condiments on the formation of HCAs in cooked chicken was investigated. Chicken samples were subjected to pan-frying under controlled temperature. The levels of HCAs DMIP, MeIQx, 4,8-DiMeIQx, PhIP, harman and norharman were found to be between 0.93 and 27.52 ng g^?1, whereas IQ, MeIQ, AαC, MeAαC, Trp-P-1 and Trp-P-2 were found either below the limit of quantification or not detected in the control sample. Nevertheless, for samples cooked using food condiments, the amounts of HCAs (DMIP, MeIQx, 4,8-DiMeIQx and PhIP) were between 0.14 and 19.57 ng g^?1; harman and norharman were detected at higher concentrations up to 17.77 ng g^?1 while IQ and MeIQ were at levels below the limit of quantification; and AαC, MeAαC, Trp-P-1 and Trp-P-2 were not detected in any of the samples. The outcomes revealed that the formation of HCAs (except harman and norharman) diminished after the addition of food condiments. Edible oil contributed to the highest levels of HCA formation, followed by garlic, paprika, pepper and tomato.     

PAH Residues in Honey by Ultrasound-Vortex-Assisted Liquid-Liquid Micro-Extraction Followed by GC-FID/IT-MS

Polycyclic aromatic hydrocarbon (PAH) residue concentrations have been measured in honey samples collected on the Italian market. An ultrasound-vortex-assisted dispersive liquid-liquid micro-extraction (UVALLME) procedure coupled with a gas chromatography flame ionization detector or ion trap mass spectrometry (GC-IT/MS) is proposed for fast analysis of fluorene, phenanthrene, anthracene, fluoranthene, pyrene, chrysene, benzo(b)fluoranthene, benzo(a)pyrene, and benzoperylene. Different analytical parameters such as extraction solvent and relative volume, best extraction time, pH, NaCl concentration, and reproducibility at low and high concentrations were optimized. Under optimal conditions, the recoveries range from 95 to 107% and correlation coefficients range from 0.893 to 0.995 whereas the limits of detection (LODs) and limits of quantification (LOQs) are ≥36 and ≥41 ng g^?1 in GC-FID and 0.030 and 0.069 ng g^?1 in GC-IT/MS, respectively. The precision, expressed as relative standard deviations (RSDs), is ≤7.4 and ≤5.2% for low and high PAH concentration levels, respectively. The whole proposed methodology, demonstrated to be simple, reproducible, and sensible, has been applied to the determination of trace PAHs in five honey samples.     

Measurement of ampicillin residue levels in chicken eggs during and after medicated feed administration by LC-MS/MS

A simple and sensitive LC-MS/MS method was developed and validated for the determination of ampicillin (ABPC) in chicken eggs. Residues were extracted by reverse-phase solid-phase extraction. Chromatographic separation was performed using a reverse-phase column with an elution gradient. The limits of detection and quantification were 0.01 and 0.1 ng g^?1, respectively. For the 0.1–50 ng g^?1 concentration range, mean recovery and accuracy values were 93.9–98.5% and 100.2–118.0%, respectively. ABPC residue concentrations in eggs before, during and after 7 days of medicated feeding of maximum dosage (40 mg kg^?1 body weight day^?1) of ABPC were determined with the LC-MS/MS method. The maximum concentration of ABPC in eggs was 3.6 ± 1.7 ng g^?1 (mean ± SD) on the last day of the administration period. Residue concentrations of ABPC in eggs during and after ABPC administration were not over the Japanese maximum residue limit of 0.01 mg kg^?1.     

Determination of Triazole Fungicides in Vegetable Samples by Magnetic Solid-Phase Extraction with Graphene-Coated Magnetic Nanocomposite as Adsorbent Followed by Gas Chromatography–Mass Spectrometry Detection

A graphene-based magnetic nanocomposites (G-Fe₃O₄ MNPs) was synthesized and used as the adsorbent for the extraction of some triazole fungicides (triadimefon, paclobutrazol, hexaconazole, myclobutanil, diniconazole, propiconazole, and tebuconazole) in cucumber, cabbage, and tomato samples prior to gas chromatography–mass spectrometry detection. Various experimental parameters affecting the extraction efficiencies, such as the amount of G-Fe₃O₄ MNPs, extraction time, pH and salt concentration of the sample solution, and desorption conditions were investigated. Under the optimized experimental conditions, the enrichment factors of the method for the analytes were in the range from 461 to 697. The signal response was linear in the range of 0.5–35.0 ng g^?1 for all the analytes with the correlation coefficients ranging from 0.9810 to 0.9986. The limits of detection (S/N?=?3) of the method for the analytes were between 0.01 and 0.10 ng g^?1. The recoveries of the method for the seven triazoles were in the range from 84.4 to 108.2 % with RSDs between 3.4 and 10.6 %.     

Fusarium species identification and fumonisin production in maize kernels from Shandong Province,China, from 2012 to 2014

A total of 225 maize kernel samples were collected from Shandong Province in China from 2012 to 2014 and analysed for contamination with Fusarium spp. and fumonisins (FBs) using molecular methods and high-performance liquid chromatography with fluorescence detection. The results showed that the average incidences of Fusarium spp. in 2012, 2013 and 2014 were 23.3%, 37.1% and 36.5%, respectively, Fusarium verticillioides being 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.     

LC-TOF/MS determination of phthalates in edible salts from food markets in Korea

Residual quantities of 12 phthalates have been monitored in edible salts (raw salts, refined salts, refined salts with additives and baked salts) available in Korean food markets. Liquid–liquid extraction followed by liquid chromatography time-of-flight mass spectrometry (LC-TOF/MS) was used to analyse the samples. The method was validated and showed linear correlation (R ² > 0.996) in the range 0.5–100 ng g^?1 for all target analytes. Recoveries were 85.9–108.4%, except for diethyl phthalate (DEP). Relative standard deviations (RSDs) were 2.7–6.0% and the limits of detection (LODs) were 1.2–2.8 ng g^?1. Although the contamination of phthalates in salt would be trivial in comparison to those of other main foods and below the reference dose of the Chronic Oral Exposure recommended by US-EPA, the availability of reference data could be valuable for food chemists and salt manufacturers.