Assessment of caffeine intake in the Korean population

An improved method for the analysis of caffeine in foods by HPLC was validated by measuring several analytical parameters. The caffeine contents of 1202 products available from Korean markets were analysed. A consumption study was conducted by using data from the Korea National Health and Nutrition Examination Survey (KNHANES), 2010–12, to estimate the caffeine intakes of the Korean population. The mean intakes of caffeine from all sources in the general population and consumers were 67.8 and 102.6 mg day^?1 for all age groups, respectively. The 95th percentile intakes of the general population and consumers were 250.7 and 313.7 mg day^?1, respectively. In those aged 30–49 years, the caffeine intakes of the general population and consumers were highest at 25.5% (101.8 mg kg^?1 day^?1) and 36.6% (0.9 mg kg^?1 day^?1), respectively, compared with the maximum recommended daily intake (400 mg day^?1) for adults. In the general population, the main contributors to the total caffeine intake were carbonated beverage for the younger age groups and coffee for the adults. These data provide a current perspective on caffeine intake in the Korean population.     

Energy drink consumption and impact on caffeine risk

The impact of caffeine from energy drinks occurs against a background exposure from naturally occurring caffeine (coffee, tea, cocoa and foods containing these ingredients) and caffeinated beverages (kola-type soft drinks). Background caffeine exposure, excluding energy drinks, was assessed for six New Zealand population groups aged 15 years and over (n = 4503) by combining concentration data for 53 caffeine-containing foods with consumption information from the 2008/09 New Zealand Adult Nutrition Survey (ANS). Caffeine exposure for those who consumed energy drinks (n = 138) was similarly assessed, with inclusion of energy drinks. Forty-seven energy drink products were identified on the New Zealand market in 2010. Product volumes ranged from 30 to 600 ml per unit, resulting in exposures of 10–300 mg caffeine per retail unit consumed. A small percentage, 3.1%, of New Zealanders reported consuming energy drinks, with most energy drink consumers (110/138) drinking one serving per 24 h. The maximum number of energy drinks consumed per 24 h was 14 (total caffeine of 390 mg). A high degree of brand loyalty was evident. Since only a minor proportion of New Zealanders reported consuming energy drinks, a greater number of New Zealanders exceeded a potentially adverse effect level (AEL) of 3 mg kg^?1 bw day^?1 for caffeine from caffeine-containing foods than from energy drinks. Energy drink consumption is not a risk at a population level because of the low prevalence of consumption. At an individual level, however, teenagers, adults (20–64 years) and females (16–44 years) were more likely to exceed the AEL by consuming energy drinks in combination with caffeine-containing foods.     

Changes in theanine and caffeine contents of black tea with different rolling methods and processing stages

Theanine is a specific amino acid in tea, which has positive effects on health. Theanine contents of different grade Turkish teas, variations in the theanine content during tea processing, and the effects of different rolling processes on theanine content were determined. Theanine content of Turkish tea varying between 0.32 and 0.43 % has been reported for the first time by this study. Theanine content decreased in all processing steps from 10.0–3.42 to 7.73–3.97 mg g^?1 dw in Orthodox and Cay-Kur methods, respectively. In both methods, the highest theanine loss (almost 50 %) was observed in the withering step, which was followed by drying step. Caffeine content of Turkish tea was determined varying between 1.8 and 2.2 %. While the caffeine content increased in the withering step, it decreased in other steps. The correlation between theanine and caffeine contents was evaluated. A high correlation (R ² = 0.87) between the caffeine and theanine contents was found in teas classified by Cay-Kur method, and caffeine/theanine ratio was found to be around 5.3 in general.     

Monitoring of 29 weight loss compounds in foods and dietary supplements by LC-MS/MS

Because of the rapid growth in dietary supplement availability and public concern for weight control, the investigation of foods and various dietary supplements illegally adulterated with weight loss compounds has become increasingly important. A total of 29 weight loss compounds, including sennoside, sibutramine, ephedrine and their analogues, found to be adulterated in foods and dietary supplements were simultaneously examined by LC-MS/MS. The 188 samples were collected between 2009 and 2012 in South Korea, and method validation was performed to determine the adulterants to the weight loss compounds. LODs, LOQs and linearity ranged from 0.03 to 7.5 ng ml^?1, from 0.08 to 30.00 ng ml^?1, and from 0.990 to 0.999, respectively. The results showed that nine weight loss compounds, namely bisacodyl, desmethylsibutramine, didesmethylsibutramine, ephedrine, fluoxetine, pseudoephedrine, sennoside A, sennoside B and sibutramine, were detected in 62 of all collected samples and were found in order of frequency as follows: sibutramine, 25.7%; sennoside A, 22.9%; sennoside B, 20.0%; fluoxetine, 8.6%; desmethylsibutramine, 7.1%; bisacodyl, ephedrine, and pseudoephedrine, 4.3%; and didesmethylsibutramine, 2.9%. Sibutramine, which was the most frequently found adulterant, ranged in levels from 0.03 to 132.40 mg g^?1 (2010), from 0.88 to 76.2 mg g^?1 (2011), and from 0.07 to 0.24 mg g^?1 (2012). Although the concentrations of most compounds ranged widely, some compounds such as bisacodyl and fluoxetine were found at high concentrations in several samples.     

Consumer exposures to anthocyanins from colour additives,colouring foodstuffs and from natural occurrence in foods

Anthocyanins are responsible for the red/blue colour of grapes, currants, and other fruits and vegetables. They may also be extracted for use as colour additives (E163) or concentrated for use as colouring foods. Consumer exposures have been assessed using data on natural occurrence, use levels and frequencies from food manufacturers and European food consumption data. Intakes from natural occurrence can be up to 4 mg kg bw^?1 day^?1 at the mean and up to 17 mg kg bw^?1 day^?1 for children who are high level consumers of red/black berries and small fruits. High-level intakes for children from food colour and colouring food applications lie in the range 0.3–6.3 mg kg bw^?1 day^?1 and for adults at 0.6–2.8 mg kg bw^?1 day^?1. Exposures from food colour use and colouring foods separately or combined are therefore lower than those from natural occurrence in foods.     

Assessment of the dietary intake of propylene glycol in the Korean population

An improved method for the analysis of propylene glycol (PG) in foods using a gas chromatography-flame ionisation detector (GC-FID), with confirmation by GC-MS, was validated by measuring several analytical parameters. The PG concentrations in 1073 products available in Korean markets were determined. PG was detected in 74.1% of the samples, in a concentration range from the limit of detection (n.d., 0.39 μg ml^?1) to 12,819.9 mg kg^?1. The Korea National Health and Nutrition Examination Survey (KNHANES) 2011–2013 reported the mean intake levels of PG from all sources by the general population and consumers were 26.3 mg day^?1 (0.52 mg kg^?1 day^?1) and 34.3 mg day^?1 (0.67 mg kg^?1 day^?1), respectively. The 95th percentile intake levels of the general population and consumers were 123.6 mg day^?1 (2.39 mg kg^?1 day^?1) and 146.3 mg day^?1 (2.86 mg kg^?1 day^?1), respectively. In all groups of the general population, breads were the main contributors to the total PG intake. These reports provide a current perspective on the daily intake of PG in the Korean population.     

Unravelling a vicious circle: animal feed marketed in Costa Rica contains irregular concentrations of tetracyclines and abundant oxytetracycline-resistant Gram-positive bacteria

Diverse tetracyclines are used to prevent and control bacterial infections in livestock and farmed fish. These drugs are administered through the diet, but farmers seldom check whether feed contains antibiotic-resistant bacteria that may colonise their crops or transfer their resistance traits to species of veterinary relevance. To examine whether antibiotic dosage defines the abundance of antibiotic-resistant bacteria in animal feed, we determined the concentration of parental compounds and epimers of oxytetracycline (OTC), doxycycline, tetracycline and chlortetracycline, as well as the abundance and resistance level of OTC-resistant bacteria in samples of fish (n = 21), poultry (n = 21), swine (n = 21), and shrimp feed (n = 21) marketed in Costa Rica. Fish feed contained the highest amounts of tetracyclines (119–8365 mg kg^?1) and the largest proportion of bacteria resistant to 10 μg ml^?1 (1.8–92.4%) or 100 μg ml^?1 of OTC (12.5–63.8%). Poultry (78–438 mg kg^?1) and swine (41–1076 mg kg^?1) feed had intermediate concentrations of tetracyclines and OTC-resistant bacteria (0.2–66% and 0.3–49%, respectively), whereas shrimp feed showed the lowest amounts of tetracyclines (21.5–50.3 mg kg^?1), no OTC and no culturable OTC-resistant bacteria. In line with these results, the MIC₅₀ of OTC for 150 isolates from fish and poultry feed was > 256 µg ml^?1, while that of 150 bacteria isolated from swine feed was 192 µg ml^?1. Phenotypic tests, fatty acid profiles and proteotypic analyses by matrix-assisted laser desorption/ionisation-time of flight mass-spectroscopy revealed that most OTC-resistant isolates were Gram-positive bacteria of low G+C% content from the genera Staphylococcus and Bacillus. Clear correlations between OTC dosage and feed colonisation with OTC-resistant bacteria were seen in medicated feed for fish (r = 0.179–0.651). Nonetheless, some unmedicated feed for fish, swine and poultry contained large populations of OTC-resistant bacteria, suggesting that raw materials and manufacturing processes may also influence carriage of OTC-resistant bacteria in animal feed.     

Fluoride content of soft drinks,nectars, juices,juice drinks,concentrates, teas and infusions marketed in Portugal

A potentiometric method using a fluoride combination ion-selective electrode was validated and used to analyse 183 samples, including soft drinks, juices, nectars, juice drinks, concentrates, teas and infusions marketed in Portugal. The fluoride levels were higher in extract-based soft drinks, juice drinks and juice, with fluoride values of 0.86 ± 0.35, 0.40 ± 0.24 and 0.37 ± 0.11 mg l^?1, respectively. The lowest fluoride concentration was found in infusion samples (0.12 ± 0.01 mg l^?1), followed by teas and carbonated soft drinks with fluoride concentrations of 0.16 ± 0.12 and 0.18 ± 0.07 mg l^?1, respectively. Nectars, concentrates and juice-based drinks had similar fluoride concentrations of 0.33 ± 0.16, 0.29 ± 0.12 and 0.25 ± 0.14 mg l^?1, respectively. The fluoride concentrations in all these samples would only contribute intakes below the acceptable daily intake (ADI = 0.05 mg kg^?1 body weight day^?1), indicating that, individually, these beverages cannot induce fluoride toxicity in the population group of children.     

Determination of 4(5)-methylimidazole in carbonated beverages by isotope-dilution liquid chromatography-tandem mass spectrometry

The purpose of this study was to develop a method to quantify 4(5)-methylimidazole (4-MEI), a suspected carcinogen, in carbonated beverages by simple sample dilution and isotope-dilution reverse-phase LC-MS/MS. Isotope dilution using hexa-deuterated methylimidazole (d₆-4-MEI) was used to quantify native 4-MEI and to assess matrix effects quantitatively. The accuracy of the method was assessed by intentionally fortifying a negative control sample at three doses: low, medium and high (replicates of n = 5 each) with a known amount of 4-MEI. The respective absolute error in each case was 18.7 ± 0.7%, 14.6 ± 2.8% and 21.1 ± 9.7%. Within-day (intra-) and day-to-day (inter-) repeatability, determined as the relative standard deviation by fortifying a negative control sample (n = 5), were 9.5% and 15.4%, respectively. Average ion suppression of d₆-4-MEI in beer was 63.9 ± 3.2%, while no suppression or enhancement was seen in non-alcoholic samples. The instrument and method limit of detection were calculated as 0.6 and 5.8 ng ml^–1, respectively. 4(5)-Methylimidazole was quantified in a variety of store-bought consumer beverages and it was found that in many of the samples tested consuming a single can of beer would result in intake levels of 4-MEI that exceed the no significant risk guideline of 29 µg day^–1. Conversely, 4-MEI in the samples was orders of magnitude smaller than the European Food Safety Authority acceptable daily intake threshold value of 100 mg kg^–1 bw day^–1.     

Determination of green,blue and yellow artificial food colorants and their abuse in herb-coloured green Easter beers on tap

Beer is one of the most popular alcoholic beverages worldwide. For consumer acceptance, significant factors are its taste, flavour and colour. This study determines selected synthetic green, blue and yellow food colorants in popular Easter herb-coloured green beers on tap produced in breweries on Holy Thursday. The abuse of beer colouring with Tartrazine (E 102), Quinoline yellow (E 104), Sunset yellow (E 110), Patent blue (E 131), Indigo carmine (E 132), Brilliant blue FCF (E 133), Green S (E 142) and Fast green FCF (E 143) was assessed in 11 green beer samples purchased in local restaurants. HPLC was used for the separation and detection of artificial colorants with diode-array detection and a Chromolith Performance CN 100 × 4.6 mm column with guard pre-column Chromolith CN 5 × 4.6 mm. Separation was performed in gradient elution with mobile phase containing methanol–aqueous 2% ammonium acetate at pH 7.0. The study showed that eight beers (70%) marketed in the Czech Republic contained artificial colorants (Tartrazine and Brilliant blue FCF). The concentration of colorants found in analysed green herb-coloured beers ranged from 1.58 to 3.49 mg l^–1 for Tartrazine, 0.45–2.18 mg l^–1 for Brilliant blue, while Indigo carmine was detected only once at concentration 2.36 mg l^–1. Only three beers showed no addition of the synthetic colorants. However, the levels of artificial colorants found in beers marketed in the Czech region were very low and did not show a serious risk for consumers’ health.     

Safety assessment and single-dose toxicokinetics of the flavouring agent myricitrin in Sprague–Dawley rats

Myricitrin, a flavonol rhamnoside of myricetin extracted from the Chinese bayberry (Myrica rubra Siebold) plant, has been used in Japan since 1992 as a flavour modifier in snack foods, dairy products, and beverages. It is affirmed as generally recognised as safe (GRAS) by the US Flavour and Extract Manufacturer Association (FEMA) and is considered safe by the Joint FAO/WHO Expert Committee on Food Additives (JECFA) at current estimated dietary exposures. In anticipation of expanded marketing, 97% pure myricitrin was fed to male and female Sprague–Dawley rats at dietary concentrations of 0.5%, 1.5% and 5.0% in a 90-day toxicity study. There was increased food consumption and decreased body weight gain in males exposed to 5% myricitrin. Blood values were within laboratory reference ranges except for mean increases in basophils in low- and high-dose males and serum phosphorus in high-dose males. In the absence of abnormal clinical or histopathological changes, these changes are not considered adverse. Based on the 90-day rat toxicity study, the no observed adverse effect level (NOAEL) is 2926 mg kg^–1 day^–1 in males and 3197 mg kg^–1 day^–1 in females. Gavage administration of myricitrin resulted in blood levels of myricitrin within 1 h after single oral doses of 250, 500 or 1000 mg kg^–1 body weight, indicating direct absorption of the glycosylated form of this flavonoid. Blood levels of myricetin, a metabolite of myricitrin, were not present in rats dosed orally with 1.6 mg kg^–1 myricetin, but were present only at 12 or 24 h in one of five, in three of five, and in four of five rats dosed with 250, 500 and 1000 mg myricitrin kg^–1 body weight, respectively, possibly a result of hepatic conversion of myricitrin to myricetin and enterohepatic recirculation of the resulting myricetin. The current studies further support prior safety assessments of myricitrin as a food flavouring.     

Survey of 11 mycotoxins in wheat flour in Hebei province,China

A survey of 11 mycotoxins in 348 wheat flour samples marketed in Hebei province of China were analysed by liquid chromatography-tandem mass spectrometry, was carried out. The selected mycotoxins consisted of four aflatoxins (AFs: AFB₁, AFB₂, AFG₁ and AFG₂) and seven Fusarium toxins, i.e. deoxynivalenol (DON), nivalenol, 3-acetyldeoxynivalenol and 15-acetyldeoxynivalenol, zearalenone, Fusarenon-X and deoxynivalenol-3-glucoside. Results indicated that most of the wheat samples analysed were contaminated with mycotoxins. Wheat was most susceptible to DON (91.4% contamination), with a mean level of 240 μg kg^?1. On average the probable daily intake (PDI, expressed as µg kg^?1 body weight day^?1) of mycotoxins was within the provisional maximum tolerable daily intake (PMTDI, 2.0 µg kg^?1 of body weight day^?1) as set by the Joint FAO/WHO Expert Committee on Food Additives. Nevertheless, exposure assessment revealed that the maximum PDI of mycotoxins was 4.06 µg kg^?1 body weight day^?1, which was twice the PMTDI value. Thus, consistent monitoring is recommended, as to keep the contamination level under control.     

Dietary exposures to eight metallic contaminants of the Hong Kong adult population from a total diet study

Dietary exposures to eight metallic contaminants, aluminium (Al), antimony (Sb), cadmium (Cd), lead (Pb), methylmercury (MeHg), nickel (Ni), tin (Sn) and vanadium (V), of the Hong Kong adult population were estimated using the total diet study (TDS) approach. The estimated mean exposures of Al (0.60 mg kg^–1 bw week^–1), Sb (0.016–0.039 µg kg^–1 bw day^–1), Cd (8.3 µg kg^–1 bw month^–1), Pb (0.21 µg kg^–1 bw day^–1), MeHg (0.74 µg kg^–1 bw week^–1), Ni (3.1 µg kg^–1 bw day^–1), Sn (0.029–0.031 mg kg^–1 bw week^–1) and V (0.13 µg kg^–1 bw day^–1) were well below the relevant health-based guidance values (HBGVs) where available. However, dietary exposures to MeHg of women aged 20–49 years (child-bearing age) accounted for 150% of the provisional tolerable weekly intake (PTWI) and to Al and Cd of some high consumers were found exceeding or approaching the HBGVs. The major food contributors of MeHg were fish and seafood (90%), of Al were non-alcoholic beverages including tea (33%), and of Cd were vegetables (36%). MeHg exposure during pregnancy was a public health concern in Hong Kong due to potential health risks to the foetus. Results suggest that there is a need to continue monitoring the exposures to metallic contaminants, especially Al, Cd and MeHg, of the Hong Kong population.     

Estimation of the intake of phenol compounds from virgin olive oil of a population from southern Spain

The objective of the study was to determine the mean polyphenol composition of different varieties of virgin olive oil (VOO) habitually consumed in the region of southern Spain and to estimate the dietary exposure to olive oil polyphenols in that population. There were statistically significant differences in total polyphenols among varieties, with the Picual variety containing the largest amount with a mean value of 591.8 mg kg^–1. The main phenolic compounds found in the VOOs under study were tyrosol and hydroxytyrosol. The highest amounts of both substances were found in Picual olive oils with concentrations of 2.3–6.6 mg kg^?1. The total intake of polyphenols from VOO ranged between 8.2 mg day^–1 (SD = 4.14) for the under 19 year olds and 21.3 mg day^–1 (SD = 3) for the over 50 year olds. Some polyphenols, including tyrosol and hydroxytyrosol, were consumed principally as olive oil. The intake of these compounds in the studied population was in the range of 88.5–237.4 μg day^–1. This has particular importance as recent studies have demonstrated that hydroxytyrosol helps to improve plasma lipids levels and repair oxidative damage related to cardiovascular disease. There was a greater dietary consumption of polyphenols in olive oil among the participants who more closely followed the Mediterranean diet pattern. A higher consumption of olive oil and therefore a greater exposure to polyphenols was observed in females versus males and in participants of normal weight versus those who were overweight. The total intake of polyphenols from VOO significantly increased with higher age, reflecting the greater intake of this oil by older people, who also show a closer adherence to the Mediterranean diet. The over 50-year-old age group showed the greatest consumption of this olive oil and therefore of phenolic compounds, which are healthy protectors in the human diet that contribute to the acknowledged benefits of the Mediterranean diet.     

Development of an ultra-high-performance liquid chromatography coupled to high-resolution quadrupole-Orbitrap mass spectrometry method for the rapid detection and confirmation of illegal adulterated sedative-hypnotics in dietary supplements

A novel method using ultra-high performance liquid chromatography coupled to hybrid quadrupole-Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap) was developed and validated for the simultaneous screening, identification and quantification of sedative-hypnotics in dietary supplements. Chromatographic conditions were optimised and a full data-dependent MS² scan (MS/dd-MS²) in positive and negative ion mode was used. A single injection was sufficient to perform the simultaneous screening and identification/quantification of samples. The response showed a good linear relationship with analyte concentrations over wide ranges (e.g., 1.0–1000 ng g^–1 for diazepam) with all the determination coefficients (r²) > 0.9985. The method was validated, obtaining accuracy (intra- and inter-day) in the range of 94.5–105.3% and precision (intra- and inter-day) in the range of 0.4–8.9%, respectively. The detection limits (LODs) were in the range of 0.3–1.0 ng g^–1 for different analytes. Recoveries were performed and ranged from 74.1% to 90.2%, while all matrix effects were over the range of 85.4–93.6%. Finally, this method was used to detect sedative-hypnotics in commercial dietary supplements. Of a total of 45 batches of dietary supplements, only three batches were found to be positive samples with concentrations of diazepam, clonazepam and alprazolam at high levels (≥ 8.22 mg g^–1).     

HPLC-ESI-MS/MS assessment of the tetrahydro-metabolites of cortisol and cortisone in bovine urine: promising markers of dexamethasone and prednisolone treatment

The effects of long-term administration of low doses of dexamethasone (DX) and prednisolone (PL) on the metabolism of endogenous corticosteroids were investigated in veal calves. In addition to cortisol (F) and cortisone (E), whose interconversion is regulated by 11β-hydroxysteroid dehydrogenases (11βHSDs), special attention was paid to tetrahydrocortisol (THF), allo-tetrahydrocortisol (aTHF), tetrahydrocortisone (THE) and allo-tetrahydrocortisone (aTHE), which are produced from F and E by catalytic activity of 5α and 5β-reductases. A specifically developed HPLC-ESI-MS/MS method achieved the complete chromatographic separation of two pairs of diastereoisomers (THF/aTHF and THE/aTHE), which, with appropriate mass fragmentation patterns, provided an unambiguous conformation. The method was linear (r² > 0.9905; 0.5–25 ng ml^?1), with LOQQ of 0.5 ng ml^?1. Recoveries were in range 75–114%, while matrix effects were minimal. The experimental study was carried out on three groups of male Friesian veal calves: group PL (n = 6, PL acetate 15 mg day^–1 p.o. for 31 days); group DX (n = 5, 5 mg of estradiol (E2) i.m., weekly, and 0.4 mg day^–1 of DX p.o. for 31 days) and a control group (n = 8). Urine was collected before, during (twice) and at the end of treatment. During PL administration, the tetrahydro-metabolite levels decreased gradually and remained low after the suspension of treatment. DX reduced urinary THF that persisted after the treatment, while THE levels decreased during the experiment, but rebounded substantially after the DX was withdrawn. Both DX and PL significantly interfered with the production of F and E, leading to their complete depletion. Taken together, the results demonstrate the influence of DX and PL administration on 11βHSD activity and their impact on dysfunction of the 5-reductase pathway. In conclusion, profiling tetrahydro-metabolites of F and E might serve as an alternative, indirect but reliable, non-invasive procedure for assessing the impact of synthetic glucocorticosteroids administration.     

Comparison of multiple methods for the determination of sulphite in Allium and Brassica vegetables

Sulphites are a family of additives regulated for use worldwide in food products. They must be declared on the label if they are present in concentrations greater than 10 mg kg^–1, determined as sulphur dioxide (SO₂). The current US regulatory method for sulphites, the optimised Monier–Williams method (OMW), produces false-positive results with vegetables from the Allium (garlic) and Brassica (cabbage) genera due to extraction conditions that are thought to cause endogenous sulphur compounds to release SO₂. Recently, modifications to the OMW method (2x MW) were published that reportedly reduced this false-positive in garlic. However, no other vegetables from these genera have been investigated. In addition, an LC-MS/MS method was developed for sulphite analysis, but it has not yet been tested with these problematic matrices. Ten vegetable species were analysed using these sulphite methods (OMW titration, OMW gravimetric, 2x MW and LC-MS/MS) to determine the false-positive rate. Sulphite concentrations > 10 mg kg^–1 SO₂ were observed with the OMW analyses. The 2x MW method reduced the measured concentration in unsulphited samples to ≤ 10 mg kg^–1 SO₂ for all matrices analysed. The LC-MS/MS method showed concentrations < 10 mg kg^–1 for the Brassica samples, but only displayed a slight reduction in the Allium matrices. Spiked recovery studies were conducted to determine if these methods can detect added sulphite. The 2x MW had recoveries of 17% and 42% for water and fresh garlic, respectively, and the LC-MS/MS had recoveries of 108%, 125%, 116% and 107% for water, fresh garlic, roasted garlic, and hummus, respectively. The low recoveries of the 2x MW may indicate that sulphur compounds cannot be properly quantified with this method. The ability to eliminate false-positives will enable accurate determination of added sulphite to ensure compliance with sulphite labelling requirements.     

Parameters affecting 5-hydroxymethylfurfural exposure from beer

5-Hydroxymethylfurfural (HMF) is generated during food and beverage heating processes and/or storage. Its daily intake, estimated as 4–10 mg day^?1, is several orders of magnitude higher than other process contaminants. Beer can be of relevance to the evaluation of HMF exposure; however, the information concerning its occurrence in different types of beer and during product storage is scarce. Therefore, the major goal of this work was to assess the amounts of HMF in different commercial beers, as well as the impact of storage, to deepen knowledge about the contribution of beer to HMF exposure. Blonde beers presented a mean content of 4.29 ± 1.05 mg L^?1, which was significantly lower (P ≤ 0.05) than those obtained for amber (6.84 ± 0.75 mg L^?1) and dark beers (6.99 ± 0.52 mg L^?1). Additionally, to study kinetic of HMF formation, fresh pilsner beers were stored at 30, 40 and 50°C during 40 days; a zero-order reaction was observed. The dependence of the rate constant on temperature was described by the Arrhenius equation and calculated activation energy was 101.85 kJ mol^?1. Storage can increase drastically HMF content, which means higher exposure for consumers. Thus, beer contribution to HMF exposure should not be neglected, since the intake of 1 L of beer entails a consumption of 4–7 mg of HMF or even more, depending on storage time and temperature.     

Contamination of wines and spirits by phthalates: types of contaminants present,contamination sources and means of prevention

This research determines the concentrations of various phthalates in French wines and grape spirits marketed in Europe or intended for export. Dibutyl phthalate (DBP), diethylhexyl phthalate (DEHP) and butyl benzyl phthalate (BBP) were the most frequently detected compounds in the wines analysed. While only 15% of the samples examined contained quantifiable concentrations (> 0.010 mg kg^–1) of DEHP and BBP, 59% of the wines contained significant quantities of DBP, with a median value as high as 0.0587 mg kg^–1. Only 17% of the samples did not contain any detectable quantity of at least one of the phthalates and 19% contained only non-quantifiable traces. In the spirits analysed, DBP (median = 0.105 mg kg^–1) and DEHP (median = 0.353 mg kg^–1) were the substances measured at the highest concentrations, as well as the most frequently detected (90% of samples). BBP was present in 40% of the samples at an average concentration of 0.026 mg kg^–1. Di-isobutyl phthalate (DiBP), which is not permitted in contact with food, was found in 25% of the spirits tested. According to the specific migration limits (SML) for materials in contact with food, slightly more than 11% of the wines analysed were non-compliant, as they exceeded the SML for DBP (0.3 mg kg^–1); just under 4% were close to the SML for DEHP. Concerning spirits, 19% of the samples analysed were considered non-compliant to the SML for DBP and nearly 7% were close to the SML for DEHP. The aged grape spirits analysed were often excessively contaminated with DiBP, which is not permitted to be used in contact with food (> 0.01 mg kg^–1). A study of various materials frequently present in wineries revealed that a relatively large number of polymers sometimes contained high concentrations of phthalates. However, the epoxy resin coatings used on vats represented the major source of contamination.     

Determination of Metals and Metalloids in Wine Using Inductively Coupled Plasma Optical Emission Spectrometry and Mini-torch

In the present study, an inductively coupled plasma optical emission spectrometer ICPE-9820 with the mini-torch technology that significantly reduces the consumption of plasma gas to 7.0 L min^?1 was applied for the multielemental analysis of wine samples. Three sample preparation procedures (microwave digestion in closed vessels, acid digestion in open vessels in a water bath, both with HNO₃, and 1:10 dilution with deionized water) were compared for the determination of 15 elements in wines. In all wines analyzed, the lowest concentration was obtained for Li (0.06–0.09 mg L^?1) and the highest for K (475–995 mg L^?1). The concentration >1 mg L^?1 of B, Fe, and Na was determined in all wines analyzed by the three sample preparation procedures. The average concentrations found for the acid extracts for Al (1.31 mg L^?1) and Fe (3.40 mg L^?1) were higher in comparison to results of sample dilution (0.73 and 1.56 mg L^?1 respectively). The recoveries were between 88.2 and 110 %, 65.9 and 106 %, and 62.8 and 109 %, whereas the relative standard deviations (RSDs) varied between 0.04 and 4.62 %, 0.74 and 5.57 %, and 0.70 and 5.80 %, respectively, for the procedure of sample dilution, microwave digestion, and water bath digestion.