Pesticides in multigrains and risk assessment for Koreans by age group.

Using GC-MS/MS, 365 pesticides were analysed simultaneously in multigrains collected in the metropolitan area in 2018 and 2019. A risk assessment was performed for the detected pesticides. The limit of quantification, recovery and relative standard deviation for the pesticides ranged from 0.9-10.5 µg/kg, 70.3-89.3% and 3.0-10.3%, respectively. Among the 240 samples of multigrains, a total of 104 pesticides were detected, resulting in a detection rate of 32.9%. Out of these, 79 samples contained more than one pesticide. Risk assessment was conducted across all age groups, ranging from children to the elderly. The hazard quotient of phenothrin in glutinous rice was found to be 0.977, which was the highest in this study. However, the hazard index did not exceed 1 in any age group. These results indicated that the detected pesticides do not pose a serious public health concern. Nonetheless, regular monitoring is necessary to ascertain food safety.

Best Achievements in Clinical Medicine in Diabetes and Dyslipidemia in 2020.

Over the last two decades, our understanding of diabetes and treatment strategies have evolved tremendously, from scientific, mechanistic, and human perspectives. The categories of anti-diabetic medications expanded from a few to numerous, enabling clinicians to personalize diabetes care and treatment. Thanks to rapid growth in the field of science and medical engineering, newer treatment options are coming to the market with various advantages and disadvantages to be aware of. Therefore, clinicians should rapidly adopt new trends based on guidelines and data from many clinical trials in the field of diabetes. In the treatment of dyslipidemia, trends and guidelines are changing every year, and novel therapies are being developed. In this review, we would like to summarize the major achievements in clinical medicine in 2020 in the field of diabetes mellitus and dyslipidemia.

Determination of 66 pesticide residues in livestock products using QuEChERS and GC-MS/MS.

Determinations of 66 pesticide residues in different matrices including beef, pork, chicken, eggs, and milk were conducted using GC-MS/MS combined with the quick easy cheap effective rugged safe (QuEChERS) method for sample extraction. A high linearity was achieved in the concentration range from 2.5 to 1000 µg/L (R 2 ≥ 0.99), and the limit of quantification for multi-class pesticides ranged from 0.74 to 23.1 µg/kg. The recovery ranged from 70.0 to 120%, while the reproducibility of the measurements was between 0.23 and 19.9%. Monitoring was conducted for livestock products purchased from local markets. Chlorpyrifos and fenitrothion in beef and chlorpyrifos in pork were detected below the maximum residue limits for the respective samples. No detectable residues were found in the other samples. Due to its high efficiency, reproducibility, and simple analytical operation, the proposed method can be applied to the regular monitoring of multi-residue pesticides in livestock products.

Analysis of illegal colourants (citrus red II, diethyl yellow, dimethyl yellow, metanil yellow and rhodamine B) in foods by LC-UV and LC-MS/MS.

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.

High-throughput simultaneous analysis of multiple pesticides in grain, fruit, and vegetables by GC-MS/MS.

A multi-component quantitative GC-MS/MS method for monitoring and inspecting agricultural products was developed for the simultaneous determination of 365 pesticide residues in grain, beans, fruit and vegetables. Twenty-six pesticides that have been authorised in foreign countries but not in Korea were included in the newly adapted Korean positive list system. The method was validated by analysing spiked samples at three concentrations (0.01, 0.05, and 0.1 mg/kg) for brown rice, soy beans, mandarin orange, potato and green pepper matrice, which represented grain, beans, fruit, and vegetables. More than 95% of 365 compounds satisfied the validation criteria of 70-120% recovery and ≤20% relative standard deviation obtained through the proposed simultaneous multi-component analysis. Twenty-two types of pesticides were detected in 76 food samples, whose concentrations were below the maximum residue limits. Among the newly added pesticides, lambda-cyhalothrin, an analogue of cyhalothrin, was detected in peaches. The method can be applied to the analysis and inspection of pesticide residues in domestic and imported agricultural products for safety control.

Dietary exposure assessment of synthetic food colours using analytical concentrations in Korea.

The safety of nine synthetic colour additives approved in Korea were assessed through hazard identification, hazard characterisation, exposure assessment, and risk characterisation. Hazard identification and characterisation were conducted using new risk information based on toxicology data. Exposure assessment calculated the estimated daily intake (EDI) of the nine colours. Finally, the risk was evaluated by comparing the EDIs of the colours with the acceptable daily intake (ADI). 1,114 samples (24 food categories) among a total of 1,454 samples contained colour additives either at a level that was not detectable or up to a quantified maximum of 288 mg kg-1. The likelihood of risk of exposure to all food colours, evaluated by comparing the EDI with the ADI, was less than 0.52% of the ADI for the general population. These results indicate that use of synthetic food colour in Korea is safe and does not result in excessive exposure to any population group.

HS-GC/MS method development and exposure assessment of volatile organic compounds from food packaging into food simulants.

A simultaneous headspace-gas chromatography/mass spectrometry (HS-GC/MS) method was developed and validated to determine the migration of 12 volatile organic compounds (methanol, acetone, methylethylketone, ethylacetate, isopropylalcohol, benzene, toluene, ethylbenzene, xylene, cumene, propylbenzene, and styrene) from food contact materials into food simulants (water, 4% acetic acid, 50% ethanol, and n-heptane). The limits of detection and quantification were 0.007-0.201 mg L-1 and 0.023-0.668 mg L-1, respectively. The method was applied to 205 samples of paper/paperboard, polyethylene, polypropylene, polystyrene, and polyethylene terephthalate. The estimated daily intake (EDI) was calculated using the migration results. Exposure assessments were carried out to compare the EDI to the tolerable daily intake (TDI); the results indicated that the EDI of styrene represented only a small percentage (8.0%) of the TDI. This analytical method will be a useful tool to examine levels of various volatile compounds migrating from food packaging to food simulants using HS-GC/MS method.

Safety assessment of antioxidants and color fixatives for the Korean population using dietary intake monitoring.

Food additives such as antioxidants and color fixatives are substances used in food intentionally for technical effect, such as decolorizing or intensifying the color of food. Based on the necessity of re-evaluating food additives for safety and to improve consumer perception, we conducted safety assessments for food additives according to the Risk Assessment Guidelines of the Korean Ministry of Food and Drug Safety. These safety assessments evaluated new risk information based on toxicology data and estimates of dietary intake exposures to food additives in comparison with the acceptable daily intake (ADI). Estimated daily intakes (EDI) of food additives were calculated using food consumption data for the Korean population derived from the Korea National Health and Nutrition Examination Survey and monitoring data based on the analysis of food additives in food products. Unlike contaminants, antioxidants and color fixatives are purposely added as food additives, and they are largely consumed in processed foods. Therefore, EDI was compared with ADI to investigate the likelihood of potentially hazardous effects in humans. The risk likelihoods of food additives, evaluated by comparing the EDI with the ADI, were less than 2% in the total population. Thus, exposure levels to antioxidants and color fixatives do not exceed the ADI. Based on the safety assessments conducted in this study, we estimate exposure to food additives to be within safe limits for all population groups.

Naturally occurring benzoic, sorbic, and propionic acid in vegetables.

Benzoic, sorbic and propionic acid are used as preservatives in foods and can also be naturally present in processed foods. The levels of preservatives in 939 vegetables were determined. Benzoic and sorbic acid were analysed by high-performance liquid chromatography with a diode-array detector and further confirmed by liquid chromatography-tandem mass spectrometry, whereas propionic acid was analysed using a gas chromatography-flame ionization detector and further confirmed by gas chromatography-mass spectrometry. Benzoic and propionic acid were found in 10.9% and 36.2%, respectively, of the samples. In contrast, sorbic acid was not found in any of the samples. The highest amounts of benzoic and propionic acid were found in perilla leaves (0.33-298 mg kg-1) and ginseng (

Simultaneous determination of sodium iron chlorophyllin and sodium copper chlorophyllin in food using high-performance liquid chromatography and ultra-performance liquid chromatography-mass spectrometry.

A simultaneous method for analyzing sodium iron chlorophyllin (SIC) and sodium copper chlorophyllin (SCC) using high-performance liquid chromatography was developed. This method employed an Inertsil ODS-2 column and diode array detection at 395 nm, using methanol-water (97:3 and 80:20, v/v) containing 1% acetic acid as the mobile phase. Liquid chromatography-tandem mass spectrometry was used to identify the main components of SIC and SCC as Fe-isochlorine e4 and Cu-isochlorine e4, respectively. The limits of detection and quantitation of SIC were 1.2 and 4.1 mg/kg, respectively, while those of SCC were 1.4 and 4.8 mg/kg, respectively. For intraday and interday tests, the SIC recoveries from candy ranged from 81% to 101%, while SCC recoveries ranged from 100% to 109%. The developed method can be applied to the rapid determination of SIC and SCC in candy.

Migration of lead and arsenic from food contact paper into a food simulant and assessment of their consumer exposure safety.

Paper is one of the most commonly used food packaging materials. During the production of packaging paper, it is possible for trace amounts of heavy metals to be incorporated as contaminants. These could migrate into food when packaging paper (food contact paper) is used for cooking, storing and eating. The aim of this study was to determine the migration of lead (Pb) and arsenic (As) from food contact paper into a food simulant and then to assess human safety through the estimated daily intake (EDI) with consumption factor. Migration tests were conducted for 310 samples using 4% acetic acid as a food simulant at 25°C for 10 min and at 95°C for 30 min. Concentrations of Pb and As in a food simulant were quantified by inductively coupled plasma mass spectrometry. LODs for Pb and As were 0.002 and 0.005 µg L-1, respectively. The migration of Pb from food contact paper ranged from not detected (ND) to 17.5 µg L-1 at 25°C for 10 min and from 0.10 to 25.6 µg L-1 at 95°C for 30 min while As ranged from ND to 0.44 µg L-1 at 25°C for 10 min and from ND to 0.87 µg L-1 at 95°C for 30 min. The migration of Pb and As determined in this study confirm that the human exposure was within safe levels based on the EDI of food contact paper compared with the provisional tolerable weekly intake for Pb of 25 µg kg-1 bw and for As of 15 µg kg-1 bw.

Migration study of caprolactam from polyamide 6 sheets into food simulants.

Caprolactam, used in manufacturing polyamide (PA) 6, may threaten human health. Here, PA 6 sheets were produced by using a twin-screw extruder to evaluate its safety. Caprolactam migration concentrations from the PA 6 sheets into food simulants were evaluated according to the standard migration test conditions under the Korean Food Standards Codex (KFSC). Concentrations were investigated under various food simulants (distilled water, 4% acetic acid, 20 and 50% ethanol, and heptane) and storage conditions (at 25, 60, and 95 °C). Caprolactam migration concentrations into food simulants were determined as follows: 4% acetic acid (0.982 mg/L), distilled water (0.851 mg/L), 50% ethanol (0.624 mg/L), 20% ethanol (0.328 mg/L), and n-heptane (not detected). Migrations were determined to be under the regulatory concentration (15 mg/L) according to the KFSC test conditions. Taken together, these results verified that the standard migration test conditions by KFSC were reliable to evaluate the safety of PA 6.

Release of N-nitrosamines and N-nitrosatable substances from baby bottle teats and rubber kitchen tools in Korea.

Ensuring the safety of baby bottle teats and kitchen tools made from rubber is critical. Therefore, the migration of N-nitrosamines and N-nitrosatable substances from 30 teats and 45 kitchen tools to artificial saliva was analyzed by liquid chromatography-tandem mass spectrometry. The method was validated by assessing the limits of detection (0.46-3.87 µg/kg), limits of quantification (1.38-11.73 µg/kg), and recoveries (86.3-108.6%) of seven compounds. Nitrosodimethylamine (NDMA), N-nitrosopiperidine, and N-nitrosomorpholine (NMOR) migrated from baby bottle teats at concentrations of not detected (ND) to 3.67 µg/kg. NDMA and NMOR concentrations ranged from ND to 1.72 µg/kg after migration from 45 rubber kitchen tools. N-nitrosatable substances ranged from ND to 42.16 µg/kg after migration from baby bottle teats but did not migrate from rubber kitchen tools. All tested products were considered safe for use, as N-nitrosamine and N-nitrosatable substance levels did not exceed the permitted management specifications.

Simultaneous analysis and exposure assessment of migrated bisphenol analogues, phenol, and p-tert-butylphenol from food contact materials.

A simple, rapid, and novel liquid chromatography tandem-mass spectrometry (LC-MS/MS) method was developed and validated to determine levels of eight bisphenol analogues (A, S, F, B, P, AF, AP, and Z), phenol, and p-tert-butylphenol migrated from food contact material (FCM) into food simulants. Method validation showed acceptable values in terms of linearity, precision, and accuracy. The limits of detection and quantification were 0.53-29.6 and 1.77-29.6 µg L-1, respectively. Water, 4% acetic acid, 50% ethanol, and n-heptane were employed as food simulants for the migration tests, and the proposed method was applied to 234 articles of 11 FCMs including polycarbonate, polyethersulfone, polypropylene, and polyethyleneterephthalate, obtained from domestic markets and manufacturers in Korea. Only phenol was found in the FCMs poly(cyclophexane-1,4-dimethylene terephthalate), polylactide, and thermoplastic polyurethane. Eight bisphenol analogues and p-tert-butyl phenol were not found in any samples. Using the obtained migration results, the estimated daily intake (EDI) of phenol was calculated. Exposure assessments were carried out to compare the EDI with the tolerable daily intake (TDI), showing a low percentage (0.18%) of the TDI reported. This is the first study to examine eight bisphenol analogues and two phenols simultaneously in FCMs using the LC-MS/MS.

Perfluorinated compounds in food simulants after migration from fluorocarbon resin-coated frying pans, baking utensils, and non-stick baking papers on the Korean market.

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.

Improved method for the determination of 12 non-nutritive sweeteners and monitoring in various foods using liquid chromatography-tandem mass spectrometry.

An improved and highly sensitive method was developed and validated for the determination of 12 (7 permitted and 5 non-permitted in Korea) non-nutritive sweeteners in various foods using liquid chromatography-electrospray ionisation-tandem mass spectrometry. The chromatographic separation was performed on an Xbridge BEH C18 column (3 mm × 100 mm, 2.5 µm) with gradient elution using 10 mM ammonium acetate in water and 10 mM ammonium acetate in methanol. Sample preparation consisted of simple dilution, homogenisation, centrifugation and purification with a C18 cartridge prior to analysis. The relative matrix effect (%ME) was within ±20% for all sweeteners. The method also showed good linearity (R2 > 0.99). The limit of detection and limit of quantification values in sample were in the range of 0.02-2.66 and 0.06-8.05 mg kg-1, respectively. The recoveries at three concentration levels ranged between 80% and 119%, with relative standard deviation values below 10%. In addition, the expanded uncertainties determined for 12 sweeteners in 5 different food matrices were confirmed to be <14%. Finally, the method was successfully applied to the analysis of sweeteners in 681 food samples purchased in Korea, Australia and Turkey. These results demonstrate that the method is suitable for the simultaneous determination of multiple-sweeteners in a variety of foods.

Fast and simple determination and exposure assessment of bisphenol A, phenol, p-tert-butylphenol, and diphenylcarbonate transferred from polycarbonate food-contact materials to food simulants.

Polycarbonate (PC) plastics find extensive use in baby bottles, food storage containers, and various kitchen items. Possibly hazardous chemicals, bisphenol A (BPA), phenol, p-tert-butylphenol (TBP), and diphenylcarbonate (DPC), are source materials or by-products from PC production. Therefore, a fast and simple analytical method was developed to determine and assess the exposure of BPA, phenol, TBP, and DPC transferred from PC food-contact materials to four different food simulants (water, 4% acetic acid, 50% ethanol, and n-heptane) at different temperatures. The method was validated in terms of limit of detection (LOD) and quantification (LOQ), recovery, and precision for the detection of BPA, phenol, and TBP using HPLC-FLD and of DPC using HPLC-UV. BPA, phenol, TBP, and DPC concentrations transferred from 200 PC samples to food simulants were determined. The highest migration levels of BPA (54.3 µg L-1) and phenol (43.8 µg L-1) were found in 50% ethanol at 70 °C. TBP did not migrate to any simulant. DPC did not show any migration from PC samples into water and only migrated from a cup to 4% acetic acid at 70 °C and 100 °C, whereas migration occurred from several cups, ladles, spoons, and tongs to 50% ethanol and to n-heptane at 25 °C. Food simulants and temperature were the crucial factors for the migration of BPA and phenol from PC samples. Estimated daily intakes (EDIs), based on food consumption and food-type distribution factors, for BPA, phenol, and DPC were calculated to be 0.007, 0.001, and 2.5 × 10-4 µg kg-1 bw day-1, respectively.

Sorbic, benzoic and propionic acids in fishery products: a survey of the South Korean market.

This study was conducted to provide basic data as part of a project to distinguish naturally occurring organic acids from added preservatives. Accordingly, we investigated naturally occurring levels of sorbic, benzoic and propionic acids in fish and their processed commodities. The levels of sorbic, benzoic and propionic acids in 265 fish and their processed commodities were determined by high-performance liquid chromatography-photodiode detection array (HPLC-PDA) of sorbic and benzoic acids and gas chromatography-mass spectrometry (GC/MS) of propionic acid. For propionic acid, GC-MS was used because of its high sensitivity and selectivity in complicated matrix samples. Propionic acid was detected in 36.6% of fish samples and 50.4% of processed fish commodities. In contrast, benzoic acid was detected in 5.6% of fish samples, and sorbic acid was not detected in any sample. According to the Korean Food and Drug Administration (KFDA), fishery products and salted fish may only contain sorbic acid in amounts up to 2.0 g kg-1 and 1.0 g kg-1, respectively. The results of the monitoring in this study can be considered violations of KFDA regulations (total 124; benzoic acid 8, propionic acid 116). However, it is difficult to distinguish naturally generated organic acids and artificially added preservatives in fishery products. Therefore, further studies are needed to extend the database for distinction of naturally generated organic acids and added preservatives.

Development and validation of HPLC method for the determination of ferrocyanide ion in food grade salts.

A rapid, simple, and reliable HPLC method was developed and validated to determine the presence of ferrocyanide ions (FeCNs) in food grade salts. An analytical column coupled with a guard column and mobile phase comprised of sodium perchlorate and sodium hydroxide (NaOH) were employed at a detection wavelength of 221nm. Samples were dissolved in 0.02M NaOH solution and filtered. For processed salts including herbs and spices, a C18 cartridge was applied to minimize interference from salt matrices. The method validation was based on linearity, accuracy (recovery), precision, LOD, LOQ, and measurement uncertainty. This method exhibits good linearity from 0.1-10mg/L (r2=0.9999). The LOD and LOQ values were determined to be 0.02 and 0.07mg/kg, respectively. The FeCN recoveries in six salt matrices ranged from 80.3-102.2% (RSD=0.3-4.4%). These results indicate that the proposed method is suitable for FeCN ion determination in various food grade salts.

Safety assessment of 16 sweeteners for the Korean population using dietary intake monitoring and poundage method.

A sweetener is a food additive that imparts a sweet taste to food products. Sweeteners have been increasingly used in Korea since the approval of sodium saccharin and d-sorbitol in 1962. Unlike food contaminants, humans are exposed to food additives only through the consumption of processed food products. For exposure assessments of sweeteners, the dietary intakes of food products containing acesulfame-K, aspartame, saccharin-Na, and sucralose were determined, and the resulting calculated estimated daily intake (EDI) values were compared directly with each additive's ADI. The poundage method was used to calculate the daily intake per capita for 12 additional sweeteners, such as lactitol, for which appropriate analytical methods for food products do not exist. The risk, as evaluated by comparing the EDI with the ADI, was determined to be 2.9% for acesulfame-K, 0.8% for aspartame, 3.6% for saccharin-Na, 4.3% for steviol glycosides, and 2.1% for sucralose. No hazardous effect was predicted for the other 11 sweeteners, including lactitol.