• Journal of Food Hygiene and Safety
• /
• v.25 no.4
• /
• pp.388-394
• /
• 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
• /
• v.35 no.3
• /
• pp.243-251
• /
• 2020

In this study, we investigated pesticide residues in 207 agricultural products distributed by direct trade in the northern area of Gyeonggi Province. A total of 94 general agricultural products and 113 eco-friendly agricultural products collected from local grocers and cooperative stores were analyzed by multiresidue method for 263 pesticides using GC (gas chromatography)/ECD (electron capture detector), GC/NPD (nitrogen phosphorus detector), GC-MS/MS (tandem mass spectrometry), LC (liquid chromatography)/PDA (photodiode array detector), LC/FLD (fluorescence detector), LC-MS/MS. All samples showing pesticide residues were general agricultural products collected from local food stores. The pesticide residue levels of 14 samples (6.8%) were below the maximum residue limits (MRLs) and one of them (0.5%) exceeded the MRLs. Sixteen pesticides were detected from samples of the following produce items: spinach, young cabbage, perilla leaves, mallow, cucumber, chives and water dropwort. The safety of the detected pesticides was assessed by monitoring the daily intake estimate (EDI) and the daily intake allowance (ADI) based on the amount of pesticides detected. The ADI percentage range (the ratio of EDI to ADI) was 0.0134-61.6259% and there was no health risk connected with consuming agricultural products in which pesticide residues were detected.

• Korean Journal of Food Science and Technology
• /
• v.39 no.2
• /
• pp.114-121
• /
• 2007

The purpose of this study was to investigate 253 kinds of pesticide residues in 58 commercial dried agricultural products in Seoul. The determinations of the pesticide residues were performed using multiresidue methods and were carried out by a gas chromatography-nitrogen phosphorus detector (GC-NPD), an electron capture detector ($GC-{\mu}ECD$), a mass spectrometry detector (GC-MSD) and high performance liquid chromatography-ultraviolet detector (HPLC-UV), and a fluorescence detector (HPLC-FLD). The pesticide residue detection rate in the commercial dried agricultural products was 24.1% (14 of 58 samples). Twelve pesticide residues without maximum residue limits (MRLs) were detected. In the vegetable groups, the frequency of pesticide residues was found to be in the increasing order of dried fruiting vegetables > dried leafy vegetables > dried stalk and stem vegetables. The pesticides used on dried red pepper in the dried fruiting vegetables were varied (7 kinds) and numerous (4 of 8 samples). The pesticide types detected in the commercial dried agricultural products were in the order of pyrethroid > organochloride > organophosphorus and insecticide > fungicide > herbicide ${\cdot}$ nematicide. The primary pyrethroid pesticide detected was cypermethrin. According to the producing areas of products, large numbers of pesticide residues were found in the order of Korea, China, North Korea, USA, and Vietnam.

• Analytical Science and Technology
• /
• v.28 no.5
• /
• pp.323-330
• /
• 2015

Alkaptonuria, a rare inherited metabolic disease, is characterized by a lack of homogentisate dioxygenase and accumulation of homogentisic acid (HGA), leading to homogentisic aciduria, arthritis, and ochronosis. In this study, a rapid analytical method, without an expensive and tedious solid phase extraction step, was developed to quantify HGA in plasma using GC-MS. HGA-spiked pooled plasma samples were subjected to liquid-liquid extraction (LLE) with ethyl acetate, followed by trimethylsilyl derivatization (TMS) and GC-MS quantification using selected ion monitoring. The formation of TMS derivative of the 1 carboxylic and 2 hydroxyl functional groups was performed by reacting BSTFA (with 10% TMCS) for 5 min at 80 ℃. For selected ion monitoring, quantification and confirmation ions were determined based on specific ions (m/z 384, m/z 341 and m/z 252) of the TMS derivative of HGA. Calibration curves of pooled normal plasma specimens showed a linear relationship in the range of 1-100 ng/µL. The precision and accuracy were within a relative standard deviation (RSD) of 1 to 15% and a bias of -5 to 25%. Recoveries were obtained in the range of 99-125% and 95-115% for intra-day and inter-day assay, respectively, at 2, 20 and 80 ng/µL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.4 ng/µL and 4 ng/µL, respectively. No homogentisic acid was excreted from normal Korean plasma samples. Collectively, the results from the present study suggest that this method could be useful for routine diagnosis and therapeutic monitoring of alkaptonuria patients with excellent sensitivity and rapidity.

• Korean Journal of Environmental Agriculture
• /
• v.36 no.2
• /
• pp.87-96
• /
• 2017

BACKGROUND: The objective of this study was to identify and compare the main phenolic compounds (anthocyanins, flavonoids, phenolic acids) in blueberry and black raspberry cultivated in Korea using ultra-performance liquid chromatography diode array detection-quadrupole time-of-flight mass spectrometry (UPLC-DAD-QTOF/MS). METHODS AND RESULTS: Twenty-nine flavonoids were identified by comparison of ultraviolet and mass spectra with data in a chemical library and published data. Blueberry contained flavonols including kaempferol, quercetin, isorhamnetin, myricetin, and syringetin aglycones. Isorhamnetin 3-O-robinobioside, kaempferol 3-O-(6"-O-acetyl)glucoside, quercetin, quercetin 3-O-arabinofuranoside (avicularin), quercetin 3-O-(6''-O-malonyl) glucoside, and quercetin 3-O-robinobioside were detected for the first time in blueberry. The flavonoids in raspberry consisted of quercetin aglycone and its glycosides. The mean total flavonoid content in blueberry [143.0 mg/100 g dry weight (DW)] was 1.5-times that in raspberry (95.4 mg/100 g DW). The most abundant flavonoid in blueberry was quercetin 3-O-galactoside (hyperoside, up to 76.1 mg/100 g DW) and that in raspberry was quercetin 3-O-glucuronide (miquelianin, up to 55.5 mg/100 g DW). Miquelianin was not detected in blueberry. CONCLUSION: Flavonol glycosides were the main flavonoids in blueberry and black raspberry cultivated in Korea. The composition and contents of flavonoids differed between blueberry and black raspberry, and may be affected by the cultivar and cultivation conditions.

• Analytical Science and Technology
• /
• v.33 no.3
• /
• pp.151-158
• /
• 2020

Alcohol, which can easily be obtained in the same way as ordinary beverages, is harmful enough to cause death due to excessive drinking and chronic alcohol intake, so it is important to maintain a proper amount of drinking and healthy drinking habits. In addition, the incidence of behavioral disturbances and impaired judgments that can be caused by chronic alcohol drinking of more than adequate amounts of alcohol is also significant. Accordingly it is very useful for forensic science to check whether the person involved is drunken or is alcoholism state in various accidents. Currently, in Korea, alcohol consumption is determined by detecting the level of alcohol or alcohol metabolism 'ethyl glucuronide (EtG)' in blood or urine samples. However, analysis of alcohol or EtG in blood or urine can only provide information about the current state of alcohol consumption because of a narrow window of detection time. Therefore, it is important to analyze the EtG as a long-term direct alcohol metabolite bio-marker in human hair and to investigate relationship between alcohol consumption and EtG concentration for the evaluation of chronic ethanol consumption. In this study, we established an analytical method for the detection of EtG in Korean hair efficiently and validated selectivity, linearity, limits of detection (LOD), limits of quantification (LOQ), matrix effect, recovery, process efficiency, accuracy and precision using liquid chromatography tandem mass spectrometry (LC-MS/MS). In addition, the assay performance was evaluated in Korean social drinker's hair and the postmortem hair of a chronic alcoholism. The results of this study can be useful in monitoring the alcohol abuse of Korean in clinical cases and legal procedures related to custody and provide a useful tool to evaluate postmortem diagnosis of alcoholic ketoacidosis in forensics.

• Korean Journal of Environmental Agriculture
• /
• v.14 no.1
• /
• pp.97-108
• /
• 1995

Nitrate concentration and ${\delta}^{15}N$ value in the groundwater in Miyakojima Island, Okinawa, were measured during 1992-1993. Water from the shallow and the deep wells at the ten separate sites were sampled. Mineral contents and natural nitrogen isotope abundance(${\delta}^{15}N$) were analyzed using a liquid chromatography and a mass spectrometry (Finnigan MAT 252). Except for waters which were directly influenced by sea water invasion, most of the groundwater showed small variations among their mineral contents and ${\delta}^{15}N$ values. The average nitrate nitrogen concentrations were $1.4{\sim}11.5mgL^{-1}$ and average ${\delta}^{15}N$ values were +4.3${\sim}$+9.7$%_o$. From the nitrate concentration and ${\delta}^{15}N$ value observed, the types of the groundwater could be categorized into four groups, such as high ${\delta}^{15}N$ and high nitrate, high ${\delta}^{15}N$ and medium nitrate, low ${\delta}^{15}N$ and medium nitrate, and low ${\delta}^{15}N$ and low nitrate, reflecting the main source of nitrate contamination, such as animal and domestic waste, animal waste and soil organic matter, soil organic matter and chemical fertilizer, and chemical fertilizer, respectively. It was discussed that the lowest ${\delta}^{15}N$ value was higher than the ${\delta}^{15}N$ value of the chemical fertilizers used in this island(-3.9${\sim}$-1.4$%_o$), then considerable amounts of nitrogen must be lost by ammonium evaporation or denitrification after fertilization.

• Korean Journal of Environmental Agriculture
• /
• v.32 no.3
• /
• pp.224-230
• /
• 2013

BACKGROUND: Perchlorate(${ClO_4}^-$) is an anion that is extremely water-soluble and environmentally stable. It mostly exists in the form of sodium perchlorate, ammonium perchlorate and potassium perchlorate which are used in rocket fuels, propellants, ignitable sources, air bag inflation systems and explosives. Perchlorate can be taken into the thyroid glands and interfere with iodide uptake. The determination of perchlorate in agricultural products is important due to its potential health impact on humans. The objective of this study was to determine the perchlorate concentrations in the samples of various agricultural products and soils. METHODS AND RESULTS: In this study, samples of cereal(Rice, Barley, Corn, Bean), vegetable(Spinach, Lettuce, Sesame, Chives, Chili, Pumpkin, Tomato), fruit(Apple, Pear, Tangerine, Grape) were analyzed for perchlorate contents. Perchlorate concentrations were analyzed by liquid chromatography-tandem mass spectrometry. The results showed that agricultural products respectively contained perchlorate concentrations in the range of : cereals N.D.~$7.46{\mu}g/kg$, vegetables $0.52{\sim}23.06{\mu}g/kg$, fruits $0.19{\sim}2.66{\mu}g/kg$. Bioconcentration factor was in the order of : vegetables > cereals > fruits. Bioconcentration factor was highest follwed by Sesame 37.88, Corn 21.51, Spinach 10.57, Tangerine 4.39, Chives 2.89 and Lettuce 1.90. The recoveries of perchlorate from spiked agricultural products and soils ranged from 87.72~111.26% and 102.09~111.23%. CONCLUSION(S): The health risk assessment results obtained in this study are lower than the RfD(Reference Dose, 0.0007 mg/kg/body weight/day) value as suggested by the Integrated Risk Information System(US IRIS). Our results indicate that, people currently exposed to perchlorate from agricultural products consumption are considered as safe.

• Journal of the Korean Society of Food Science and Nutrition
• /
• v.40 no.6
• /
• pp.903-911
• /
• 2011

In this study, Bacillus polyfermenticus CJ6 harboring antibacterial activity was isolated from meju. The antibacterial activity of Bacillus polyfermenticus CJ6 was stable in the pH range of 3.0~9.0, but it disappeared after culture at $70^{\circ}C$ for 24 hr. Antibacterial activity was inactivated by proteinase K, protease, and ${\alpha}$-chymotrypsin, indicating its proteinaceous nature. The growth inhibitory effects of B. polyfermenticus CJ6 culture on food-borne pathogens such as Staphylococcus aureus, Salmonella Typhi, Listeria monocytogenes, and Escherichia coli O157:H7 were examined in this study. Approximately 6~6.2 log CFU/mL of each pathogen was co-cultured with B. polyfermenticus CJ6 in a 50 mL culture volume for 24 hr. Growth of S. aureus and L. monocytogenes was completely inhibited after 3 hr of incubation. Growth of S. Typhi and E. coli O157:H7 was also completely inhibited after 6 hr of incubation. The antibacterial compounds from B. polyfermenticus CJ6 were purified by solid phase extraction (C18 Sep-pak cartridge), recycling preparative HPLC, and analytical HPLC. Ultra-high performance liquid chromatography and electrospray ionization tandem mass spectrometry analysis were used to identify the purified antibacterial compounds, which were confirmed to be five peptides (757.4153 Da, 750.3444 Da, 1024.5282 Da, 1123.6083 Da, and 1617.8170 Da).

• Journal of Food Hygiene and Safety
• /
• v.31 no.2
• /
• pp.94-98
• /
• 2016

This study was conducted to establish the simultaneous analysis method for veterinary drug residues in honey by high performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS). The eleven targeting veterinary drugs with honey test method in Korean Food Standards Codex were divided into Group 1 (streptomycine dihydrostreptomycine, neomycine) and Group 2 (oxytetracycline, enrofloxacin, ciprofloxacin, cymiazole, chloramphenicol, amitraz, coumaphos, fluvalinate) to be analyzed simultaneously. From the results, the retention time (RT) of the targeting drugs was within 15 min, the range of detection limits was 0.0056 to $0.0643{\mu}g/g$ and the range of quantification limits was 0.0169 to $0.1948{\mu}g/g$. The coefficients of determination ($R^2$) for Group 1 ($0.05{\sim}1.0{\mu}g/mL$) and Group 2 ($0.01{\sim}1.0{\mu}g/mL$) were 0.9917~0.9987 and 0.9923~1.000 respectively, and showed the good linearity. The recovery rates for Group 1 (final conc. $0.25{\mu}g/g$) and Group 2 (final conc. $1.0{\mu}g/g$) were 65.1~80.6% and 64.2~90.3% respectively. Also, the analysis results of inter day (n = 3) and intra day (n = 6) RSD (%) for area and retention time showed that the RSD (%) for area and retention time was below 10.92% and 1.57%. Therefore, the simultaneous analysis method of this study is evaluated to be a good test method for veterinary drug residues in honey.