While the use of food additives is common manufacturing practice, the levels used in food have to be compliant with the prescribed legislation. For fast control of present levels of food additives in products, ultra-high performance liquid chromatography coupled to tandem mass spectrometry with a triple quadrupole linear ion trap (QTRAP) mass analyser was applied to develop a method for the simultaneous determination of 41 frequently added food additives and flavourings, including 16 water-soluble colourants, 14 illegal dyes, 7 sweeteners, 2 preservatives, and 2 purine alkaloids. The method was validated using energy drink, chilli powder, condiment, and jelly sweets as food sample matrices. The average recovery values were in the range of 70‒120%, and the relative standard deviations were less than 10% for the majority of the analytes. The validated method was applied for the analysis of 134 samples from the Czech market.
Titanium dioxide (TiO2), an E171 manufacturer-made food additive, is extensively utilised as a colourant in drug and a food products. Some studies showed that most of confectionary and food items contain inexplicable particles. The aim of this article is to determine the size and structure of TiO2 nanoparticles in different food products. Ten food samples, including coffee cream, white chocolate concentrate, frosting, gum, yoghurt candy, hard candies and chewy candies, were investigated for this purpose. The crystalline structure and particle size of TiO2 were determined by Powder X-ray Diffraction (PXRD) and Transmission Electron Microscopy (TEM). TEM images revealed that a few of the extracted nanoparticles had a rod-like shape, but most were spherical. Also, the size of the TiO2 particle had a wide distribution between 12 and 450 nm. Thus, to avoid human health risk, crucial factors such as size, and shape should be considered and regulated by food authorities.
Titanium dioxide (TiO2) is commonly used in foods with code E171. There is information on the food packaging that it contains E171 in the ingredients section. However, there is no information on the amount of E171 used as ingredient. Therefore, determination of TiO2 content of foods is extremely important for human health. In this study, confectionary foods, chewing gums, chocolates and white colored foods were investigated. TiO2 levels of investigated foods were determined by inductively coupled plasma optical emission spectrometry (ICP-OES). The average titanium dioxide concentrations were found ranging from 3 to 2400 mg kg-1. The size of TiO2 particles in the foods samples was determined with transmission electron microscopy (TEM). Titanium dioxide nanoparticles in the studied foods were found to vary in size from 30 to 410 nm.
Per- and polyfluoroalkyl substances (PFAS) are persistent environmental pollutants linked to various health risks. This study assessed PFAS contamination in commonly consumed food items in Luxembourg and evaluated potential dietary exposure. Between 2022 and 2024, a number of 204 samples of animal- and non-animal origin were analysed. At least one regulated PFAS compound was quantified in 48 samples (23%). Perfluorooctanoic acid (PFOA) and perfluorooctane sulphonic acid (PFOS) were the most frequently quantified compounds, found in 34 and 25 samples, respectively. The highest levels occurred in wild boar (1.14 µg/kg) and egg samples (0.21 µg/kg), while plant-based foods showed generally lower levels. Two samples (plums and potatoes) exceeded the indicative PFOA level of 0.01 µg/kg outlined in Commission Recommendation (EU) 2022/1431. PFAS intake from analysed commodities did not indicate a health risk for the general population, though hunters and frequent game (especially boar) consumers may experience elevated exposure.
Aluminium (Al) levels of 90 food samples were investigated. Nineteen samples contained Al levels exceeding the tolerable weekly intake (TWI) for young children [body weight (bw): 16 kg] when consuming two servings/week. These samples were purchased multiple times at specific intervals and were evaluated for Al levels. Al was detected in 27 of the 90 samples at levels ranging from 0.01 (limit of quantitation) to 1.06 mg/g. Of these, the Al intake levels in two samples (cookie and scone mix, 1.3 and 2 mg/kg bw/week, respectively) exceeded the TWI as established by European Food Safety Authority, although the level in the scone mix was equivalent to the provisional TWI (PTWI) as established by Joint Food and Agriculture Organization of the United Nations/World Health Organization Expert Committee on Food Additives. The Al levels markedly decreased in 14 of the 19 samples with initially high Al levels. These results indicated reductions in the Al levels to below the PTWI limits in all but two previously identified food samples.
Endocrine disrupting chemicals (EDCs) such as per- and polyfluoroalkyl substances (PFAS), bisphenols, and parabens are used in food packaging or as preservatives and their unintended consumption has been associated with cancer and other diseases. Food EDCs data are scarce in Malaysia. Thus, liquid chromatography mass tandem spectrometry (LC-MS/MS) was utilised to analyse 18 EDCs from different food categories. Bisphenol was the most abundant EDC found, followed by PFAS and paraben. Bisphenol levels in canned foods, dairy products, canned drinks, fruits, and vegetables ranged from 1.16 to 183 ng/g. PFAS was found in almost every food category, with canned foods having the highest concentrations (0.18-34.5 ng/g). Only canned foods, fruits, and vegetables contained parabens, with mean concentrations ranging from 0.27 to 26.7 ng/g. PFOS, PFBA, PFHQA and bisphenol A all had hazard quotients (HQ) above 1, indicating that they can pose a risk to human health.
This study determines the occurrence and concentration levels of artificial low-calorie sweeteners (LCSs) in food and food supplements on the Italian market. The analysed sample set (290 samples) was representative of the Italian market and comprised of beverages, jams, ketchups, confectionery, dairy products, table-top sweeteners and food supplements. All samples were analysed via UPLC-MS/MS. The method was in-house validated for the analysis of seven LCSs (aspartame, acesulfame-K, saccharin, sucralose, cyclamate, neotame and neohesperidin dihydrochalcone) in food and for five LCSs (aspartame, acesulfame-K, saccharin, cyclamate and sucralose) in food supplements. Except for cyclamate in one beverage which exceeded the maximum level (ML) with 13%, all concentrations measured in food were around or below the ML. In food supplements, 40 of the 52 samples (77%) were found to be above the ML, with exceedances of up to 200% of the ML.
This study investigated fluorinated pesticide residues in food commodities marketed in Luxembourg, focusing on substances listed in the European Chemicals Agency's Annex XV Restriction Report Proposal as potential precursors of trifluoroacetic acid (TFA), a persistent degradation product of concern. From 6,034 samples collected between 2011 and 2024, 48.1% contained quantifiable residues, with fluorinated compounds detected in 12.3% of the samples. Tea (65.3%) and dried fruits (45.6%) showed the highest contamination rates. Detection rates of fluorinated pesticide residues rose from 9.6% of the samples in 2011 to 26.8% in 2024. In 18 cases (1.8%) EU maximum residue limits (MRLs) were exceeded. Thirty-one distinct fluorinated pesticides were identified, with six compounds, fluopyram, lambda-cyhalothrin, trifloxystrobin, bifenthrin, fluopicolide, and flonicamid accounting for nearly 80% of the detections, all being considered potential precursors of TFA. These findings underline the need for continued monitoring and regulatory attention to limit environmental and health risks from TFA formation.
An analytical method was developed for investigating aminocarminic acid occurrence in E120-labelled red-coloured-beverages and in E120 additives, with the aim of controlling the purity of the carmine additive in countries where the use of aminocarminic acid is forbidden. The carminic acid and the aminocarminic acid were separated by high-performance liquid chromatography-photodiode array-tandem mass spectrography (HPLC-PDA-MS/MS). The method was statistically validated. The regression lines, ranging from 10 to 100 mg/L, showed r(2 )> 0.9996. Recoveries from 97% to 101% were obtained for the fortification level of 50 mg/L; the relative standard deviations did not exceed 3%. The LODs were below 2 mg/L, whereas the LOQs did not exceed 4 mg/L. The method was successfully applied to 27 samples of commercial E120-labelled red-coloured beverages and E120 additives, collected in Italy during quality control investigations conducted by the Ministry. The results demonstrated that more than 50% of the samples contained aminocarminic acid, evidencing the alarming illicit use of this semi-synthetic carmine acid derivative.
Perfluorinated compounds (PFCs) are used in manufacturing food contact materials, including non-stick cookware coatings and oil- and moisture-resistant paper coatings. The chemical stability of PFCs poses an issue for human safety, as they do not degrade well naturally and hence may accumulate in the body. In terms of food safety, since dietary intake is thought to be a major source of exposure to PFCs, it is necessary to assess the migration of PFCs from food packaging articles to food under typical cooking and storage conditions. An analytical method was developed for assessing the migration of 16 PFCs from food contact materials to food simulants using liquid chromatography-tandem mass spectrometry. The applicability of the method for regular inspection was assessed by monitoring 312 samples. Based on the results of the exposure assessment, all food contact materials deemed to be safe for use, which evaluated migrated concentrations and dietary food intake.
Upward trend in the use of food supplements urged the assessment of their safety. Eighty-eight liquid herbal supplements collected in Novi Sad (Serbia) in 2018 (36 samples) and 2021 (52 samples) were analysed for the presence of benzoates and sorbates (HPLC-UV) and benzene (HS-GC/MS). Benzoic acid varied from 599 to 9253 mg/kg and sorbic acid between 185 and 1658 mg/kg. The acceptable daily intake of sorbic acid was not reached, but in case of benzoic acid, it was exceeded by 5.3% of the samples. The presence of benzene was confirmed in 41.2% of benzoate preserved supplements (0.9-51.7 µg/kg). Benzene exposure revealed no health concern: maximum hazard quotients ranged from 0.39% (toddlers) to 0.84% (adolescents); minimum margins of exposure were between 35,680 (adolescents) and 77,419 (toddlers); estimates of lifetime cancer risk did not reach one extra cancer case per 100 000 persons. However, measures to mitigate benzene presence in food should be considered.
This study was designed to investigate the occurrence and exposure assessment of multiple mycotoxins in corn-based food products from Shandong Province, China. Results demonstrated that the mean level of total mycotoxins in test samples was 197.2 µg/kg. The most frequently found mycotoxins were deoxynivalenol (96.7%) and fumonisin B1 (94.4%), with mean contamination levels of 65.24 and 128.2, respectively. Among these corn-based food products, thin corn pancake had the highest mean contamination (886.7 µg/kg), followed by wotou (143.7 µg/kg), corn cake (135.4 µg/kg) and mantou (63.73 µg/kg). The average exposure values to total fumonisins and deoxynivalenol were 0.05 and 0.02 µg/kg bw/day, which were lower than the provisional maximum tolerable daily intake values of 2 and 1 µg/kg bw/day, respectively, as established by the Joint FAO/WHO Expert Committee on Food Additives. In the future strict control and systematic monitoring are needed to secure food safety and human health.
This study aimed to examine the levels of sodium benzoate (SB), potassium sorbate (PS), and natamycin (NAT) in doogh samples collected during the winter and summer in Sulaymaniyah, Kurdistan region of Iraq, utilising high-performance liquid chromatography with UV detection (HPLC-UV). Moreover, human health risks associated with these preservatives in doogh were assessed using Monte Carlo simulations. SB, PS, and NAT levels in the doogh ranged from <0.47 to 22.5 mg/L, <0.015 to 8.3 mg/L, and 1.4 to 11.5 mg/L, respectively. The levels of these preservatives in the doogh samples were within international standards. The estimated daily intake (EDI) values of SB, PS, and NAT in doogh were below the acceptable daily intake (ADI). Hazard quotient (HQ) data of SB and PS in doogh were below 1. Based on these findings, the obtained levels of preservatives in doogh do not pose a health risk to Iraqi consumers.
This study analysed the physicochemical properties of 93 different meat product samples from the Kosovo market, focusing on the critical examination of nitrite and chloride levels to assess food safety and public health implications. The samples involved fresh and minimally processed meats, cooked meat products, cured meats, and traditional sausages, adhering to ISO standard methodologies for assessing pH, water activity, sodium chloride and nitrite concentrations. The survey revealed that while nitrite levels in meat products comply with EU safety regulations, sodium chloride content in certain products, particularly sausages and dry cured meats, is significantly higher than recommended. Frequent consumption of these high-salt products may lead to excessive sodium intake among consumers. These findings underscore the need for regular monitoring of sodium chloride levels in meat products, implementation of sodium-reduction strategies by meat producers, and enhanced consumer education on health risks associated with high sodium intake.
Saffron solutions, saffron rice and saffron chicken samples were considered for synthetic colours as additives, which are forbidden according to Iranian national standards. Samples were taken from restaurants of three locations and analysed by high-performance liquid chromatography. Of the total 573 samples, 52% were positive for at least one colour. The most prevalent colours were Tartrazine, Quinoline Yellow and Sunset Yellow, with 44%, 9.1% and 8.4% of the samples testing positive for these colours, respectively. Carmoisine and Ponceau were both detected only in 0.5% of the positive samples and found only in saffron solution. In conclusion, synthetic food colours, especially Tartrazine should be regarded as a potential risk in saffron and its related food. Therefore, new attempts for food safety and quality should be undertaken to eliminate the use of these colours in restaurants.
Coccidiostats are widely used as feed additives to prevent coccidiosis. The off-label use of anticoccidials or feeding non-target animals with cross-contaminated feedingstuffs may result in the occurrence of coccidiostat residues in animal tissues and eggs. In EU countries, food of animal origin is subjected to official control of residues according to Council Directive 96/23/EC. In Poland, within the framework of the National Residue Control Plan, 3718 samples (3533 targeted and 185 suspect) of animal liver, eggs, drinking water and feed were tested for coccidiostats between 2007 and 2010. Violative residues of nicarbazin, lasalocid, maduramicin, salinomycin, semduramicin and robenidine were detected in 77 food samples (53 samples of chicken liver, 23 samples of eggs and 1 sample of turkey liver). A high percentage (31%) of non-compliant feed samples collected during follow-up investigations was observed, which confirms that feed cross-contamination may be the reason of the occurrence of coccidiostat residues in food.
Synthetic colourants are highly regulated due to their correlation with a variety of health hazards. Regulatory services must be able to detect the substances in a cost-effective, efficient, and sensitive manner. LC-UV and LC-MS/MS methods have been developed to simultaneously detect five illegal colourants in foods, such as: citrus red II, diethyl yellow, dimethyl yellow, metanil yellow, and rhodamine B. This method showed good linearity (R 2 > 0.99) and low limits of detection (0.09-0.19 mg kg-1) and quantitation (0.26-0.58 mg kg-1). The recoveries at three standard concentration levels ranged between 80.9% and 120%, with relative standard deviations below 12%. The expanded uncertainties determined for the five colourants in three food matrices were 8.2-19.4%. This method was applied to monitor five illegal colourants in imported and domestic beverages, candies, and sauces. None of the five colourants were found in any of the 510 samples. The method is suitable for quantitative analysis of five illegal colourants simultaneously in various foods and can be applied to improve current surveillance and inspection services.
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 (R² > 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.
Some synthetic dyes are fraudulently added into spices to appeal visually to consumers. Food regulations in several countries, including the United States, Australia, Japan and the European Union, strictly prohibit the use of unauthorised synthetic dyes in food. Nevertheless, illegal practices persist, where spices contaminated with potentially carcinogenic dyes have been documented, posing potential health risks to consumers. In the present study, 14 synthetic dyes were investigated through liquid chromatography/tandem mass spectrometry in 252 commercially available spices in the Singapore market. In 18 out of these (7.1%) at least 1 illegal dye was detected at concentrations ranging from 0.010 to 114 mg/kg. Besides potential health risks, presence of these adulterants also reflects the economic motivations behind their fraudulent use. Findings in the present study further emphasise the need for increased public awareness, stricter enforcement, and continuous monitoring of illegal synthetic dyes in spices to ensure Singapore's food safety.