Dietary exposure of Hong Kong adults to fatty acid esters of 3-monochloropropane-1,2-diol

A total of 290 individual food samples were collected in Hong Kong, China, for 3-monochloropropane-1,2-diol (3-MCPD) fatty acid esters analysis. Most samples were processed food and in ready-to-eat form. The results show that the levels of 3-MCPD fatty acid esters were high in biscuits, fats and oils, snacks and Chinese pastry with mean bound 3-MCPD levels of 440, 390, 270 and 270 μg kg^?1, respectively. The dietary exposures to bound 3-MCPD of average and high adult consumers were estimated to be 0.20 and 0.53 μg kg bw^?1 day^?1, respectively. The primary toxicological concern of 3-MCPD fatty acid esters is its potential to release 3-MCPD in vivo during digestion in the gastrointestinal tract. 3-MCPD would affect the kidney, the central nervous system and the male reproductive system of rats. Assuming that 100% of the 3-MCPD was released from 3-MCPD fatty acid esters by hydrolysis in the digestive system, the dietary exposures to 3-MCPD for average and high adult consumers were only 10% and 26% of the provisional maximum tolerable daily intake (PMTDI) of 3-MCPD established by the Joint Food and Agriculture Organization/World Health Organization Expert Committee on Food Additives (JECFA) (2 μg kg bw^?1 day^?1), respectively. The results suggest that both average and high adult consumers are unlikely to experience major toxicological effects of 3-MCPD.     

3-Monochloropropane-1,2-diol fatty acid esters in commercial deep-fat fried foods

Levels of 3-monochloropropane-1,2-diol (3-MCPD) fatty acid esters were evaluated in commercial deep-fat fried foods from the Brazilian market using a GC-MS method preceded by acid-catalysed methanolysis. A limit of detection of 0.04 mg kg^?1, a limit of quantitation of 0.08 mg kg^?1, mean recoveries varying from 82% to 92%, and coefficients of variation ranging from 2.5% to 5.0% for repeatability and from 3.6% to 6.5% for within-laboratory reproducibility were obtained during in-house validation. The levels of the compounds in the evaluated samples, expressed as free 3-MCPD equivalent, ranged from not detected to 0.99 mg kg^?1, and the highest concentrations were observed in samples of chopped onion and garlic. A preliminary estimation of 3-MCPD intake using these occurrence data suggested low risks to human health, but a potential concern may arise in particular cases of consumers of fried food.     

Occurrence of 3-MCPD fatty acid esters in human breast milk

A series of twelve breast milk samples were analysed by gas chromatography-mass spectrometry (GC/MS) operated in selected ion monitoring mode for 3-chloropropane-1,2-diol (3-MCPD). Whilst none of the samples contained 3-MCPD above the limit of detection of 3 μg kg^?1 milk, all contained high amounts of 3-MCPD esterified with higher fatty acids. The levels of 3-MCPD released by hydrolysis of these esters (bound 3-MCPD) ranged from the limit of detection (300 μg kg^?1, expressed on a fat basis) to 2195 μg kg^?1; with a mean level of bound 3-MCPD of 1014 μg kg^?1, which corresponded to 35.5 μg kg^?1 milk. The presence of bound 3-MCPD was confirmed using orthogonal gas chromatography coupled with high-speed time-of-flight mass spectrometry analysis for four randomly selected breast milk samples. Six breast milks collected from one of the nursing mothers 14–76 days after childbirth contained bound 3-MCPD within the range of 328–2078 μg kg^?1 fat (mean 930 μg kg^?1 fat). The calculated bound 3-MCPD content of these samples was within the range of 6 and 19 μg kg^?1 milk (mean of 12 μg kg^?1 milk). The major types of 3-MCPD esters were the symmetric diesters with lauric, palmitic, and oleic acids, and asymmetric diesters with palmitic acid/oleic acid among which 3-chloro-1,2-propanediol 1,2-dioleate prevailed.     

Occurrence of bound 3-monochloropropan-1,2-diol content in commonly consumed foods in Hong Kong analysed by enzymatic hydrolysis and GC-MS detection

The aim of this study was to determine the level of bound 3-monochloropropan-1,2-diol in foodstuffs commonly consumed in Hong Kong, China, by an enzymatic hydrolysis indirect method which proved to be free from interferences. A total of 290 samples were picked up randomly from the local market and analysed. About 73% of these samples were found to contain detectable amounts of bound 3-MCPD. Amongst the 73 food items, bound 3-MCPD was not detected in 13 food items, including extra virgin olive oil, beef ball/salami, beef flank, ham/Chinese ham, nuts, seeds, soy sauce, oyster sauce, butter, yoghurt, cream, cheese and milk. For those found to contain detectable bound 3-MCPD, the content ranged up to 2500 µg kg^?1. The highest mean bound 3-MCPD content among the 14 food groups was in biscuits (440 [50–860] µg kg^?1), followed by fats and oils (390 [n.d.–2500] µg kg^?1), snacks (270 [9–1000] µg kg^?1), and Chinese pastry (270 [n.d.–1200] µg kg^?1). Among the samples, the highest bound 3-MCPD content was in a grape seed oil (2500 µg kg^?1), followed by a walnut flaky pastry (1200 µg kg^?1) and a grilled corn (1000 µg kg^?1). Basically, the results of this study agreed well with other published results in peer-reviewed journals, except for cheese, cream, ham, nuts and seeds.     

Occurrence of 3-MCPD and glycidyl esters in edible oils in the United States

Fatty acid esters of 3-monochloropropanediol (3-MCPD) and glycidol are processing contaminants found in a wide range of edible oils. While both 3 MCPD and glycidol have toxicological properties that at present has concerns for food safety, the published occurrence data are limited. Occurrence information is presented for the concentrations of 3-MCPD and glycidyl esters in 116 retail and/or industrial edible oils and fats using LC-MS/MS analysis of intact esters. The concentrations for bound 3-MCPD ranged from below the limit of quantitation (<LOQ) to 0.09 mg kg^?1 (ppm) in 22 unrefined oils and from 0.005 to 7.2 mg kg^?1 (ppm) in 94 refined oils. The concentrations for bound glycidol ranged from <LOQ to 0.03 mg kg^?1 (ppm) in unrefined oil samples and from <LOQ to 10.5 mg kg^?1 (ppm) in processed oil samples. The highest concentrations for both 3-MCPD and glycidol were seen in refined palm oil and palm olein samples. Palm olein samples also contained a higher percentage of 3-MCPD in mono-ester form than any other type of oil.     

Migration studies of 3-chloro-1,2-propanediol (3-MCPD) in polyethylene extrusion-coated paperboard food packaging

The manufacturing process of paperboard food packaging can produce small quantities of 3-chloro-1,2-propanediol (3-MCPD or 3-monochloropropane-1,2-diol) when wet-strength resins containing epichlorohydrin are used. 3-MCPD is from the same family as 1,3-dichloro-2-propanol (1,3-DCP), which is known to cause cancer in animals. 3-MCPD has been found in acid hydrolyzed vegetable protein, Asian sauces and paperboard for food contact. In this investigation, we conducted extraction studies to measure 3-MCPD migration into food simulant solvents from the food contact side of polyethylene extrusion-coated paperboard beverage cartons and aqueous extractions of cut pieces from the entire paperboard. We demonstrate that 3-MCPD confirmed present at concentrations up to 9.9 mg kg^?1 within the paperboard matrix does not migrate through the polyethylene-coated food contact surface. The aqueous extraction of the entire paperboard and food contact side extractions with aqueous/acidic food simulants were performed using US Food and Drug Administration (FDA) and European Commission (EU) migration testing protocols. We also show that no significant amount of 3-MCPD migrates through the unskived edges on the inside seam of the paperboard structure. The methodology for the aqueous and migration cell extractions using GC–MS analyses was validated with a limit of quantification (LOQ) of 0.009 mg kg^?1 and a limit of detection (LOD) of 0.005 mg kg^?1.     

Co-occurrence of aflatoxins,ochratoxin A and citrinin in “egusi” melon (Colocynthis citrullus L.) seeds consumed in Ireland and the United Kingdom

The natural co-occurrence of aflatoxins (AFs), ochratoxin A (OTA) and citrinin (CIT) in melon seed samples obtained from retailers and households in Ireland and the United Kingdom (UK) was evaluated. AFs and OTA were determined by HPLC with fluorescence detection while CIT was analysed by HPLC-MS/MS. AFB₁ was detected in all (100%) samples (mean = 9.7 μg kg^?1; range = 0.2–66.5 μg kg^?1). Mean total AFs was 12.0 μg kg^?1 (range = 0.3–82 μg kg^?1). Commercially retailed samples showed a significantly higher AFB₁ contamination (p < 0.05) than the household samples. OTA occurred in 3 (13.6%) samples, while 4 (18.2%) were contaminated with CIT at very low levels. In this study, 68% of the melon seed samples were contaminated above the 2 μg kg^?1 EU limit for AFB₁ in oilseeds. These results highlight the need for the development of strategies to reduce AF contamination in “egusi” for human consumption.     

Polycyclic aromatic hydrocarbons in Italian preserved food products in oil

A method based on gas chromatography/ tandem mass spectrometry was used to assess levels of 16 EU priority polycyclic aromatic hydrocarbons (PAHs) in 48 preserved food products in oil including foods such as vegetables in oil, fish in oil and oil-based sauces obtained from the Italian market. The benzo[a]pyrene concentrations ranged from <0.04 to 0.40 µg kg^?1, and 72.9% of the samples showed detectable levels of this compound. The highest contamination level was observed for chrysene with three additional PAHs (benzo[a]anthracene, benzo[b]fluoranthene and benzo[c]fluorene) giving mean values higher than the mean value for benzo[a]pyrene. Chrysene was detected in all the samples at concentrations ranging from 0.07 to 1.80 µg kg^?1 (median 0.31 µg kg^?1). The contamination expressed as PAH4 (sum of benzo(a)pyrene, chrysene, benzo(a)anthracene and benzo(b)fluoranthene), for which the maximum tolerable limit has been set by Commission Regulation (EU) No. 835/2011, varied between 0.10 and 2.94 µg kg^?1.     

Occurrence of patulin and 5-hydroxymethylfurfural in apple sour,which is a traditional product of Kastamonu,Turkey

Apple sour is a traditional product of Kastamonu, Turkey. It is consumed by spreading on bread or drinking after diluting with water. The aim of this study was to determine patulin (PAT) and 5-hydroxymethylfurfural (HMF) in apple sour. This study is the first to evaluate the occurrence of PAT and HMF in apple sour. The samples were extracted with ethyl acetate using liquid-liquid extraction technique. PAT and HMF were determined by HPLC with UV detection. PAT was detected in all samples, and the PAT level in 94.9% of samples was found to be equal or greater than the legal limit for juice concentrates. The mean value for PAT was found to be 284 ± 307 μg kg^?1. PAT levels in 13 of 39 samples were in the range of 100 ≤ x < 200 μg kg^?1, two samples were in the range of 0 ≤ x < 50 μg kg ?1 and two samples were in the range of 1000 ≤ x < 1500 μg kg¹. HMF levels of all samples were above the legal limit for solid molasses. The mean value for HMF was found to be 16215 ± 13317 mg kg^?1. HMF levels of 10 of 39 samples were determined to be in the range of 10000 ≤ x < 20000 mg kg^?1, eight samples were in the range of 20000 ≤ x < 30000 mg kg^?1 and only three samples were in the range of 100 ≤ x < 1000 mg kg^?1. There was a significant and inverse relationship between HMF and pH of the samples. These results indicate that consumption of apple sour is a considerable risk in terms of HMF and PAT toxicity.     

Polyether ionophores residues in Minas Frescal cheese by UHPLC-MS/MS

ABSTRACT

An analytical method was developed and validated for the determination of three polyether ionophores (monensin, lasalocid, and salinomycin) in 60 samples of Brazilian Minas Frescal cheese by UHPLC-MS/MS. Linearity ranged from 1 to 8 μg kg^?1 for monensin and salinomycin, and from 0.50 to 4 μg kg^?1 for lasalocid. Limits of detection and quantitation were 0.50 μg kg^?1 and 1 μg kg^?1, respectively, for both monensin and salinomycin, and 0.25 μg kg^?1 and 0.50 μg kg^?1, respectively, for lasalocid. Recoveries were between 69% and 84% with coefficients of variation up to 16.28% for repeatability and 13.79% for intermediate precision. A total of 60 samples of Minas Frescal cheese were analysed and only monensin residues were found. Monensin was detected in 55% of the samples and quantified in 5 of them at mean levels varying from 1.00 to 1.73 μg kg^?1. The proposed method demonstrated the suitability for monitoring these substances in cheese.     

3-Monochloropropane-1,2-diol (3-MCPD) in soy sauces and similar products available from retail outlets in the UK

A survey of the level of 3-monochloropropane-1,2-diol (3-MCPD) in soy sauces and similar products available in the UK is reported. The survey was carried out by the Joint Ministry of Agriculture, Fisheries and Food/Department of Health Food Safety and Standards Group (JFSSG) to check for compliance with the Food Advisory Committee's (FAC) recommended limit for 3-MCPD of 0.01mg/kg following reports that soy sauces in several European countries had been found to contain high levels (up to 124mg/kg) of 3-MCPD. Forty samples of soy sauce and similar products purchased from retail outlets were analysed using a GC-MS procedure which had been formally validated by an earlier collaborative trial. 3-MCPD was undetectable in 21 (52%) of samples analysed in the survey, with a further five samples containing very low levels of between 0.01 and 0.02mg/kg. Five samples (13%) contained 3-MCPD at levels in the range 0.020-1mg/kg while nine samples (23%) were found to contain 3-MCPD at levels greater than 1mg/kg, with the highest level being 30.5mg/kg.     

Dietary exposure to chloropropanols of secondary school students in Hong Kong

This paper reports levels of 3-monochloropropan-1,2-diol (3-MCPD) and 1,3-dichloro-2-propanol (1,3-DCP) in a wide range of food items and estimates their dietary exposure for secondary school students in Hong Kong. Dietary exposure to chloropropanols was estimated using local food consumption data obtained from secondary school students in 2000 and the concentrations of 3-MCPD and 1,3-DCP in food samples taken from the local market. The dietary exposure to 3-MCPD for an average secondary school student consumer was estimated to be 0.063–0.150 µg kg^?1 body weight (bw) day^?1, whilst that for the high consumer was 0.152–0.300 µg kg^?1 bw day^?1. Both estimates fell below the provisional maximum tolerable daily intake of 2 µg kg^?1 bw established by the Joint Expert Committee on Food Additives (JECFA) and amounted to less than 20% of this safety reference value. The dietary exposure to 1,3-DCP for an average secondary school student consumer was estimated to be 0.003–0.019 µg kg^?1 bw day^?1, whilst that for the high consumer was 0.009–0.040 µg kg^?1 bw day^?1. The resulting margins of exposures were of low concern for human health. It could be concluded that both the average and high secondary school student consumers were unlikely to experience major toxicological effects of 3-MCPD and 1,3-DCP.     

Aflatoxins and ochratoxin A in export quality raisins collected from different areas of Pakistan

During 2012–2014, 170 samples of export quality raisins were collected from different vendors in Pakistan. The collected samples were analysed for the presence of aflatoxins (AFs) and Ochratoxin A (OTA) contamination using high-performance liquid chromatography technique. The limit of detection and limit of quantification of AFs/OTA were 0.12/0.10 and 0.36/0.30 µg kg^?1, respectively. Only 5% of the samples were contaminated with AFs, ranging 0.15–2.58 µg kg^?1 with a mean of 0.05 ± 0.26 µg kg^?1. None of the raisin samples exhibited AFs contamination above the maximum limit (ML = 4 µg kg^?1) as set by the European Union (EU). About 72% of the samples were contaminated with OTA, ranging 0.14–12.75 µg kg^?1 with a mean of 2.10 ± 1.9 µg kg^?1. However, in 95.3% of the tested samples, OTA level was lower than the ML of 10 µg kg^?1 as regulated by the EU. Apparently, a strict and continuous monitoring plan, including regulatory limits, improves food safety and quality for all types of commodities.     

Aflatoxin M1 in processed milk and infant formulae and corresponding exposure of adult population in Serbia in 2013–2014

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.     

Optimization of QuEChERS Procedure Coupled to GC-ECD for Organochlorine Pesticide Determination in Carrot Samples

An optimised version of the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method for simultaneous determination of 14 organochlorine pesticides in carrots was developed using gas chromatography coupled with electron-capture detector (GC-ECD) and confirmation by gas chromatography tandem mass spectrometry (GC-MS/MS). A citrate-buffered version of QuEChERS was applied for the extraction of the organochlorine pesticides, and for the extract clean-up, primary secondary amine, octadecyl-bonded silica (C18), magnesium sulphate (MgSO₄) and graphitized carbon black were used as sorbents. The GC-ECD determination of the target compounds was achieved in less than 20 min. The limits of detection were below the EU maximum residue limits (MRLs) for carrots, 10–50 μg kg^?1, while the limit of quantification did exceed 10 μg kg^?1 for hexachlorobenzene (HCB). The introduction of a sonication step was shown to improve the recoveries. The overall average recoveries in carrots, at the four tested levels (60, 80, 100 and 140 μg kg^?1), ranged from 66 to 111 % with relative standard deviations in the range of 2–15 % (n?=?3) for all analytes, with the exception of HCB. The method has been applied to the analysis of 21 carrot samples from different Portuguese regions, and β-HCH was the pesticide most frequently found, with concentrations oscillating between less than the limit of quantification to 14.6 μg kg^?1. Only one sample had a pesticide residue (β-HCH) above the MRL, 14.6 μg kg^?1. This methodology combines the advantages of both QuEChERS and GC-ECD, producing a very rapid, sensitive and reliable procedure which can be applied in routine analytical laboratories.     

Aflatoxins and ochratoxin A: occurrence and contamination levels in cocoa beans from Brazil

In the present study, the occurrence of aflatoxins (AFs) and ochratoxin A (OTA) was evaluated in 123 samples of cocoa beans produced in five Brazilian states. The presence of these mycotoxins was determined by high-performance liquid chromatography with fluorescence detection (HPLC-FLD) after immunoaffinity column clean-up. The mean level of total AFs in cocoa beans samples was 5.7 μg.kg^?1. Four (3.3%) samples exceeded the maximum limit of 10 μg.kg^?1 established by the Brazilian legislation for total AFs. The mean level of OTA contamination was 1.2 μg.kg^?1, and none of the samples exceeded the maximum limit established by the Brazilian legislation. The co-occurrence of AFs and OTA was observed in 4.9% of the samples. The results of the present study demonstrated that, in relation to the levels of AFs and OTA established by the Brazilian legislation, most samples of cocoa beans analyzed are safe for consumption. This is the first report on the occurrence and levels of AFs and OTA in cocoa beans from the five main Brazilian states producing cocoa. The data in this study provide important information for farmers, traders, industry, consumers and law enforcement agencies.     

Determination of glyphosate,AMPA, and glufosinate in honey by online solid-phase extraction-liquid chromatography-tandem mass spectrometry

A simple method was developed for the simultaneous determination of glyphosate, its main degradation product (aminomethylphosphonic acid), and glufosinate in honey. Aqueous honey solutions were derivatised offline prior to direct analysis of the target analytes using online solid-phase extraction coupled to liquid chromatography-tandem mass spectrometry. Using the developed procedure, accuracies ranging from 95.2% to 105.3% were observed for all analytes at fortification levels of 5, 50, and 150 μg kg^?1 with intra-day precisions ranging from 1.6% to 7.2%. The limit of quantitation (LOQ) was 1 μg kg^?1 for each analyte. Two hundred honey samples were analysed for the three analytes with AMPA and glyphosate being most frequently detected (99.0% and 98.5% of samples tested, respectively). The concentrations of glyphosate were found to range from <1 to 49.8 μg kg^?1 while those of its degradation product ranged from <1 to 50.1 μg kg^?1. The ratio of glyphosate to AMPA was found to vary significantly amongst the samples where both analytes were present above the LOQ. Glufosinate was detected in 125 of 200 samples up to a maximum concentration of 33.0 μg kg^?1.     

Metal levels in Trachurus trachurus and Cyprinus carpio in Turkey

Concentrations of five toxic metals were determined in two fish species from Turkish cities during 2010–2011. The obtained lead concentrations for all of the studied Trachurus trachurus (mean 777 μg kg^?1) and Cyprinus carpio (mean 439 μg kg^?1) samples were found to be higher than the maximum level (ML) of 300 μg kg^?1, while Cd concentrations in the same samples were lower than the ML. Mean chromium (501 μg kg^?1), Ni (272 μg kg^?1) and Cu (785 μg kg^?1) concentrations in T. trachurus were significantly higher than in C. carpio (336 μg Cr kg^?1, 229 μg Ni kg^?1 and 394 μg Cu kg^?1), similar to those of Pb and Cd. Measured Pb concentrations in T. trachurus tissues are significantly higher than the ML, while those of Cd in both T. trachurus and C. carpio species were lower than the ML values.     

Aflatoxins in animal feed in Iran

One hundred and forty-six samples of animal feed (barley, n = 60; wheat bran, n = 22; wheat dry pulp, n = 29; and canola meal, n = 35) were collected in 2011 from Mashhad (Khorasan, Iran). Aflatoxins (AFs) were determined in these samples after immunoaffinity column clean-up by high-performance liquid chromatography (HPLC) with fluorescence detection. Aflatoxin B₁ (AFB₁) contamination was found in 28 samples: in five of the barley samples (8.3%) at a mean level of 0.48 µg·kg^?1, in two wheat bran samples (9.0%) at a mean level of 0.88 µg·kg^?1, in 10 wheat dry pulp samples (34.5%) at a mean level of 0.30 µg·kg^?1 and in 11 canola meal samples (31.4%) at a mean level of 0.92 µg·kg^?1. AFB₁ levels were below the maximum levels of Iran regulations (5 µg·kg^?1) and the EU maximum limit (5 µg·kg^?1).     

Aflatoxins and ochratoxin A in flour: a survey of the Serbian retail market

This report presents data on the occurrence of aflatoxins (AF) and ochratoxin A in different types of flour marketed in Serbia. A total of 114 samples of wheat, buckwheat, rye, oat, barley, rice, millet and corn flour were collected in the period 2012–2016 and analysed using high performance liquid chromatography with fluorescence detection. Among flours other than corn, AFB1 was quantified only in rice, while ochratoxin A (OTA) was found in 29% of the samples. In corn flours the percentage of positive samples varied greatly over the years: AFB1 7.1–80.0%, OTA 30.0–40.6%, with a co-occurrence of 7.1–34.4%. Overall 5.2% of flours other than corn and 10.7% of corn flours exceeded the maximum levels (MLs) for AFB1 and/or OTA. The highest recorded levels were 8.80 μg kg^?1 of AFB1 (corn) and 23.04 μg kg^?1 of OTA (rye). Overall mean contamination levels of corn flours were 0.53 μg kg^?1 of AFB1 and 0.46 μg kg^?1 of OTA.