• Horticultural Science & Technology
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• v.34 no.1
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• pp.172-182
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• 2016

This study was aimed to determine the changes in vitamin $B_5$ and $B_6$ contents compared to fresh materials after parboiling treatment of the main vegetables consumed in Korea. The specificity of accuracy and precision for vitamin $B_5$ and $B_6$ analysis method were validated using high-performance liquid chromatography (HPLC). The recovery rate of standard reference material (SRM) was excellent, and all analysis was under the control line based on the quality control chart for vitamin $B_5$ and $B_6$. The Z-score for vitamin $B_6$ in food analysis performance assessment scheme (FAPAS) proficiency test was -1.0, confirming reliability of analytical performance. The vitamin $B_5$ and $B_6$ contents in a total of 39 fresh materials and parboiled samples were analyzed. The contents of vitamin $B_5$ and $B_6$ ranged from 0.000 to 2.462 and from 0.000 to $0.127mg{\cdot}100g^{-1}$, respectively. The highest contents of vitamin $B_5$ and $B_6$ were $2.462mg{\cdot}100g^{-1}$ in fresh fatsia shoots (stem vegetables), and $0.127mg{\cdot}100g^{-1}$ in fresh spinach beet (leafy vegetables), respectively. Moreover, the vitamin $B_5$ and $B_6$ contents for parboiling treatment in most vegetables were reduced or not detected. In particular, the contents of vitamin $B_5$ in parboiled fatsia shoots and vitamin $B_6$ in parboiled yellow potato and spinach beet were decreased 20- and 4-fold compared with fresh material, respectively. These results can be used as important basic data for utilization and processing of various vegetable crops, information for dietary life, management of school meals, and national health for Koreans.

• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.13-21
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• 2019

A method was developed for the simultaneous detection of an antibiotic fungicide, streptomycin, and its metabolite (dihydrostreptomycin) in agricultural products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted using methanol adjusted to pH 3 using formic acid, and purified with a HLB (Hydrophilic lipophilic balance) cartridge. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.001 to 0.1 mg/kg, and linearity of five agricultural products (hulled rice, potato, soybean, mandarin, green pepper), with coefficients of determination $(R^2){\geq}0.9906$, for streptomycin and dihydrostreptomycin. The mean recoveries at three fortification levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) were from 72.0~116.5% and from 72.1~116.0%, and relative standard deviations were less than 12.3% and 12.5%, respectively. The limits of quantification (LOQ) were 0.01 mg/kg, which are satisfactory for quantification levels corresponding with the Positive List System. All optimized results satisfied the criteria ranges requested in the Codex guidelines and the Food Safety Evaluation Department guidelines. The present study could serve as a reference for the establishment of maximum residue limits and be used as basic data for detection of streptomycin and dihydrostreptomycin in food.

• Journal of Food Hygiene and Safety
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• v.25 no.4
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• pp.388-394
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• 2010

Metabolomics aims at the comprehensive, qualitative and quantitative analysis of wide arrays of endogenous metabolites in biological samples. It has shown particular promise in the area of toxicology and drug development, functional genomics, system biology and clinical diagnosis. In this study, analytical technique of MS instrument with high resolution mass measurement, such as time-of-flight (TOF) was validated for the purpose of investigation of amino acids, sugars and fatty acids. Rat urine and serum samples were extracted by selected each solvent (50% acetonitrile, 100% acetonitrile, acetone, methanol, water, ether) extraction method. We determined the optimized liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) system and selected appropriated columns, mobile phases, fragment energy and collision energy, which could search 17 metabolites. The spectral data collected from LC/TOFMS were tested by ANOVA. Obtained with the use of LC/TOFMS technique, our results indicated that (1) MS and MS/MS parameters were optimized and most abundant product ion of each metabolite were selected to be monitorized; (2) with design of experiment analysis, methanol yielded the optimal extraction efficiency. Therefore, the results of this study are expected to be useful in the endogenous metabolite fields according to validated SOP for endogenous amino acids, sugars and fatty acids.

• Journal of Food Hygiene and Safety
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• v.29 no.2
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• pp.131-140
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• 2014

The objective of this study was to develop a simultaneous method of 8 penicillin antibiotics including amoxicillin, ampicillin, cloxacillin, dicloxacillin, nafcillin, oxacillin, penicillin G and penicillin V in meat using LC-MS/MS. The procedure involves solid phase extraction with HLB cartridge and subsequent analysis by LC-MS/MS. To optimize MS analytical condition of 8 compounds, each parameter was established by multiple reaction monitoring in positive ion mode. The chromatographic separation was achieved on a $C_{18}$ column with a mobile phase of 0.05% formic acid and 0.05% formic acid in acetonitrile at a flow rate of 0.2 mL/min for 20 min with a gradient elution. The developed method was validated for specificity, linearity, accuracy and precision in beef, pork and chicken. The recoveries were 71.0~106%, and relative standard deviations (RSD) were 4.0~11.2%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.003~0.008 mg/kg and 0.01~0.03 mg/kg, respectively, that are below maximum residue limit (MRL) of the penicillins. This study also performed survey of residual penicillin antibiotics for 193 samples of beef, pork and chicken collected from 9 cities in Korea. Penicillins were not found in all the samples except a sample of pork which contained cloxacillin (concentration of 0.08 mg/kg) below the MRL (0.3 mg/kg).

• Journal of Food Hygiene and Safety
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• v.20 no.4
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• pp.277-283
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• 2005

A plasticizer is a substance which is added to a material to improve its processability, flexibility and stratchability. Phthalates and adipates are the most frequently used plasticizers of poly(vinyl chloride) (PVC). However, they can migtate into food from PVC food packaging, and some of them are especially suspected as endocrine disruptors. In this study, Simultaneous analysis of 13 phthalates and 9 adipates were carried out by dual-column gas chromatography system equipped wi two FID detectors for rapid confirmation and quantification. The Proposed method was validated with > 0.993 of linearity in the ranges of 10-500 mg/l, < $3.5\%$ RSD of reproducability in 10 inter-days sample preparations, and > $98.1\%$ of recoveries for all the plasticizers. DEHA was detected in all the 3 PVC wraps at levels of 176.9-198.5mg/g. Among the 51 samples of PVC gaskets, the targeted plasticizers were detected in 41 samples. Of these plasticizer detected samples,40 contained DIDP at the levels of 157.3-374.7 mg/g and one contained DMP at the levels of 165.6 mg/g. Also, some plasticizers were detected in other packaging materials such as PET, PP, PE, Pulp. But it might be attributed to contamination in manufacturing.

• Journal of Food Hygiene and Safety
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• v.31 no.4
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• pp.227-249
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• 2016

Arsenic and its compounds vary in their toxicity according to the chemical forms. Inorganic arsenic is more toxic and known as carcinogen. The provisional tolerable weekly intake (PTWI) of $15{\mu}g/kg$ b.w./week established by the Joint FAO/WHO Expert Committee on Food Additives (JECFA) has been withdrawn, while the EFSA panel suggested $BMDL_{0.1}$ $0.3{\sim}8{\mu}g/kg\;b.w./day$ for cancers of the lung, skin and bladder, as well as skin lesions. Rice, seaweed and beverages are known as food being rich in inorganic arsenic. As(III) is the major form of inorganic arsenic in rice and anaerobic paddy soils, while most of inorganic arsenic in seaweed is present as As(V). The inorganic arsenic in food was extracted with solvent such as distilled water, methanol, nitric acid and so on in heat-assisted condition or at room temperature. Arsenic speciation analysis was based on ion-exchange chromatography and high-performance liquid chromatography equipped with atomic absorption spectrometry and inductively coupled plasma mass spectrometry. However, there has been no harmonized and standardized method for inorganic arsenic analysis internationally. The inorganic arsenic exposure from food has been estimated to range of $0.13{\sim}0.7{\mu}g/kg$ bw/day for European, American and Australian, and $0.22{\sim}5{\mu}g/kg$ bw/day for Asian. The maximum level (ML) for inorganic arsenic in food has established by EU, China, Australia and New Zealand, but are under review in Korea. Until now, several studies have conducted for reduction of inorganic arsenic in food. Inorganic arsenic levels in rice and seaweed were reduced by more polishing and washing, boiling and washing, respectively. Further research for international harmonization of analytical method, monitoring and risk assessment will be needed to strengthen safety management of inorganic arsenic of foods in Korea.

• Journal of Food Hygiene and Safety
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• v.33 no.3
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• pp.176-184
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• 2018

The aim of the present work was to develop simultaneous methods of quantification of carazolol, azaperone, and azaperol residues in livestock and fishery products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Samples were extracted from beef, pork, chicken, egg, milk and shrimp using acetonitrile (ACN); while flat fish and eel were extracted using 80% ACN. For purification, ACN saturated n-hexane was used to remove fat composition. The standard calibration curves showed good linearity as correlation coefficients; $r^2$ was > 0.99. Average recoveries expressed were within the range of 67.9-105% for samples fortified at three different levels ($0.5{\times}MRL$, $1{\times}MRL$ and $2{\times}MRL$). The correlation coefficient expressed as precision was within the range of 0.55-7.93%. The limit of quantification (LOQ) was 0.0002-0.002 mg/kg. The proposed analytical method showed high accuracy and acceptable sensitivity based on Codex guideline requirements (CAC/GL71-2009). This method can be used to analyze the residue of carazolol, azaperone, and azaperol in livestock and fishery products.

• Food Science and Preservation
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• v.24 no.7
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• pp.983-991
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• 2017

This study was performed to update the National Standard Food Composition Table (NSFCT) published by Korea Rural Development Administration, especially focusing on vitamin $B_{12}$ for Korean pork. Total 7 primal and 22 retail fresh cuts of Korean pork were analyzed for vitamin $B_{12}$ and the applied immunoaffinity-HPLC was validated. Vitamin $B_{12}$ assay by immunoaffinity-HPLC obtained recoveries over 95% and coefficient variations of precision below about 10%, which met the limits required for validation acceptance. Limits of detection and quantification of immunoaffinity-HPLC were 0.01 and $0.33{\mu}g/100g$, respectively. Quality control chart showed that analysis performance was excellent during the entire of study. Vitamin $B_{12}$ contents of pork cuts significantly varied depending the types of primal and its retail cuts (p<0.05). Belly, Boston butt, rib cuts showed relatively high vitamin $B_{12}$ contents compared to other primal cuts. Vitamin $B_{12}$ content of pork retail cuts were also significantly different within the same primal cuts (p<0.05). Among 22 retail cuts, the highest vitamin $B_{12}$ was observed in Tosisal in belly primal part ($0.98{\mu}g/100g$) while both Aldeungsimsal in loin and Hongdukkaesal in hide leg were the lowest by $0.33{\mu}g/100g$. This study provides reliable vitamin $B_{12}$ data for the Korean pork fresh cuts through standard sampling, method validation and analytical quality control, which would be used for update of Korean NSFCT.

• Journal of Applied Biological Chemistry
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• v.64 no.2
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• pp.113-119
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• 2021

Olive (Olea europaea L.) leaves, a raw material for health functional foods and cosmetics have abundant polyphenols including oleuropein (major bioactive compound) with various biological activities: antioxidant, antibacterial, antiviral, anticancer activity, and inhibit platelet activation. Oleuropein has been reported as skin protectant, antioxidant, anti-ageing, anti-cancer, anti-inflammation, anti-atherogenic, anti-viral, and anti-microbial activity. Despite oleuropein is the important compound in olive leaves, there is still no quantitative approach to reveal oleuropein content in commercial products. Therefore, a validated method of analysis has to develop for oleuropein. In this study, the components and oleuropein content in 10 types of products were analyzed using a developed method with ultra-performance liquid chromatography to quadrupole time-of-flight mass spectrometry, charge of aerosol detector, and photodiode array. The total of 18 compounds including iridoids (1, 3, 4, 14, and 16-18), coumarin (2), phenylethanoids (5, 9, and 11), flavonoids (6-8, 10, 12, and 13), lignan (15), were tentatively identified in the leaves extract based high resolution mass spectrometry data, and the content of oleuropein in each product was almost identical between two detection methods. The oleuropein in three commercial product (A, G, H) was contained more over the suggested content, and it of five products (B, E, H, I, J) were analyzed within 5-10% error range. However, the two products (C, D) were found far lower than suggested contents. This study provides that analytical results of oleuropein could be a potential information for the quality control of leaf extract for a manufactured functional food.

• Journal of Food Hygiene and Safety
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• v.28 no.3
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• pp.247-251
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• 2013

The objective of present study was to develop a simultaneous determination method of 5 medical compounds, including beclomethasone, dexamethasone, prednisolone, ketoprofen, phenylbutazone in foods, using LC-MS/MS. To optimize MS analytical condition of 5 compounds, each parameter was established by MRM mode. The chromatographic separation was achieved on a C18 column successfully, with a mobile phase made up of A (0.1% formic acid) and B (0.1% formic acid in acetonitrile), at a flow rate of 0.3 mL/min for 17 min with a gradient elution. LOD and LOQ of 5 compounds were in the range of 0.40~4.60 ng/mL and 0.81~11.46 ng/mL, respectively. As a result of analyzing the three concentrations of the standard mixture added to blank samples, the results showed that the mean recovery rate of 5 compounds was in the range of 81.52~103.83%, and RSD (%) of Intra- and Inter-day assay were 0.52-10.45. Since relatively fine selectivity, accuracy and reproducibility were shown in this qualified experimental method, it could be utilized efficiently to investigating those 5 compounds to see if it is added to food products illegally.