• Journal of Food Hygiene and Safety
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• v.33 no.2
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• pp.110-117
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• 2018

The aim of this study was to develop an analytical method for the quantification of diazepam residues in fishery products, using liquid and gas chromatography-tandem mass spectrometry (LC-MS/MS and GC-MS/MS). The sample utilized in the study was extracted from the fish sample (crucian carp) using 0.1% formic acid in acetonitrile. For the utilization of the purification process, the dispersive solid phase extraction (dSPE) was used for LC-MS/MS, dSPE and SPE was used for GC-MS/MS, respectively. To be sure, the standard calibration curves showed a good linearity as the noted correlation coefficients, $r^2$ was > 0.99. The average recoveries for accuracy ranged in 99.8~124% for the samples which were fortified at three different levels (0.001, 0.002 and 0.010 mg/kg). The correlation coefficient for the precision effect was measured at a range of 4.01~11.8%. The limit of detection (LOD) for the diazepam analysis was 0.0004 mg/kg, and the limit of the quantification (LOQ) was 0.001 mg/kg. The proposed analytical method was characterized with a high accuracy and acceptable sensitivity to meet the established Codex Alimentarius Commission (CAC/GL71-2009) guideline requirements. We therefore established the optimal analysis method for the determination of diazepam in the fishery products using LC-MS/MS and GC-MS/MS. It would be applicable to analyze the diazepam residues in fishery products in further studies on this subject.

• Journal of Food Hygiene and Safety
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• v.33 no.2
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• pp.118-123
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• 2018

The objective of this study was to develop a sensitive method for the identification and determination of nitrovin in fishery products by using a solid-phase extraction (SPE), as performed with a liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with a mixture of acetonitrile and water, and were then defatted with acetonitrile saturated hexane, after which further clean-up was accomplished with SPE on the hydrophilic-lipophilic balance (HLB) cartridges. The analytes were subsequently ionized in the positive mode of an electrospray ionization (ESI), and where thereby detected in a process of multiple reaction monitoring (MRM). The linearity (expressed as correlation coefficients) of the matrix calibration curves was > 0.985. The limit of the quantification for the nitrovin was measured at 0.001 mg/kg. The accuracy (expressed as average recovery) was noted between 72.1 and 122%. The precision (expressed as coefficient variation) was noted from 2.9 to 16.9%. According to the CODEX CAC/GL-71 guideline accuracy, precision, linearity, and limit of detection were determined in three matrices (which were flatfish, eel and shrimp). The proposed method was suitable for analyzing the associated nitrovin residues. This application and result can also be a factor to contribute to the non-detection drugs management in fishery products.

• Food Science and Preservation
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• v.24 no.3
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• pp.325-333
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• 2017

This study aimed to investigate the various biological activities of Geranium thunbergii such as antimicrobial activity and protective effect against oxidative damage. To evaluate its antioxidant and antimicrobial activities, we first performed methanol extraction; this methanol extract was further partitioned using various solvents. And then, its antioxidant activity was measured using various assays including total phenolic content and protection against oxidative DNA damage, and antimicrobial activities were examined using minimum inhibiting concentration (MIC) test, and paper disc method. In addition, high-performance liquid chromatography was performed to analyze the major chemical components of ethyl acetate fraction. The G. thunbergii fraction with ethyl acetate exhibited higher antioxidant and antimicrobial activities than the other fractions. The results showed that G. thunbergii ethyl acetate fraction at $50{\mu}g/mL$ had strong DPPH and ABTS radical scavenging activities of 80.88% and 80.12%, respectively. In addition, the ethyl acetate fraction protected DNA from the oxidative damage induced by ferrous ion and hydroxyl radicals and showed high antimicrobial activity with diameter of inhibition zones ranging from 13.33 to 15.67 mm. High-performance liquid chromatography analysis revealed the major phenolic compounds of G. thunbergii to be ellagic acid and gallic acid. These results suggest that G. thunbergii might protect DNA against oxidative stress induced by reactive oxygen species and can be utilized as a natural source of antioxidant and antimicrobial agent in the food industry.

• Journal of Microbiology and Biotechnology
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• v.31 no.4
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• pp.540-549
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• 2021

The Wnt/β-catenin signaling pathway is involved in breast cancer and Myxococcus fulvus KYC4048 is a myxobacterial strain that can produce a variety of bioactive secondary metabolites. Although a previous study revealed that KYC4048 metabolites exhibit anti-proliferative effects on breast cancer, the biochemical mechanism involved in their effects remains unclear. In the present study, KYC4048 metabolites were separated into polar and non-polar (ethyl acetate and n-hexane) fractions via liquid-liquid extraction. The effects of these polar and non-polar KYC4048 metabolites on the viability of breast cancer cells were then determined by MTT assay. Expression levels of Wnt/β-catenin pathway proteins were determined by Western blot analysis. Cell cycle and apoptosis were measured via fluorescence-activated cell sorting (FACS). The results revealed that non-polar KYC4048 metabolites induced cell death of breast cancer cells and decreased expression levels of WNT2B, β-catenin, and Wnt target genes (c-Myc and cyclin D1). Moreover, the n-hexane fraction of non-polar KYC4048 metabolites was found most effective in inducing apoptosis, necrosis, and cell cycle arrest, leading us to conclude that it can induce apoptosis of breast cancer cells through the Wnt/β-catenin pathway. These findings provide evidence that the n-hexane fraction of non-polar KYC4048 metabolites can be developed as a potential therapeutic agent for breast cancer via inhibition of the Wnt/β-catenin pathway.

• Clean Technology
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• v.25 no.1
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• pp.14-18
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• 2019

In general after the etching process, waste etching solution contains metals. (ex. Nickel (Ni), Chromium (Cr), Zinc (Zn), etc.) In this work, we proposed a recycling process for waste etching solution and refining from waste liquid contained nickel to make nickel metal nano powder. At first, the neutralization agent was experimentally selected through the hydrolysis of impurities such as iron by adjusting the pH. We selected sodium hydroxide solution as a neutralizing agent, and removed impurities such as iron by pH = 4. And then, metal ions (ex. Manganese (Mn) and Zinc (Zn), etc.) remain as impurities were refined by D2EHPA (Di-(2-ethylhexyl) phosphoric acid). The nickel powders were synthesized by liquid phase reduction method with hydrazine ($N_2H_4$) and sodium hydroxide (NaOH). The resulting nickel chloride solution and nickel metal powder has high purity ( > 99%). The purity of nickel chloride solution and nickel nano powders were measured by EDTA (ethylenediaminetetraacetic) titration method with ICP-OES (inductively coupled plasma optical emission spectrometer). FE-SEM (field emission scanning electron microscopy) was used to investigate the morphology, particle size and crystal structure of the nickel metal nano powder. The structural properties of the nickel nano powder were characterized by XRD (X-ray diffraction) and TEM (transmission electron microscopy).

• Korean Journal of Environmental Agriculture
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• v.40 no.2
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• pp.134-141
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• 2021

BACKGROUND: The analytical method was established for determination of fungicide chinomethionat in several animal commodities using gas chromatography (GC) coupled with electron capture detector (ECD). METHODS AND RESULTS: In order to verify the applicability, the method was optimized for determining chinomethonat in various livestock products including beef, pork, chicken, milk and egg. Chinomethionat residual was extracted using acetone/dichloromethane(9/1, v/v) with magnesium sulfate and sodium chloride (salting outassociated liquid-liquid extraction). The extract was diluted by direct partitioning into dichloromethane to remove polar co-extractives in the aqueous phase. The extract was finally purified with optimized silica gel 10 g. CONCLUSION: The method limit of quantitation (MLOQ) was 0.02 mg/kg, which was in accordance with the maximum residue level (MRL) of chinomathionate as 0.05 mg/kg in livestock product. Recovery tests were carried out at two levels of concentration (MLOQ, 10 MLOQ) and resulted in good recoveries (84.8~103.0%). Reproducibilities were obtained (Coefficient of variation <5.2%), and the linearity of calibration curves were reasonable (r²>0.995) in the range of 0.01-0.2 ㎍/mL. This established analytical method was fully validated and could be useful for quantification of chinomathionat in animal commodities as official analytical method.

• Journal of Applied Biological Chemistry
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• v.65 no.1
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• pp.17-21
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• 2022

A new rapid and simple method for metalaxyl in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai has been developed and validated. This study was conducted to develop a method for analyzing metalaxyl by a method based on QuEChERS using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Samples were extracted with acetonitrile and purified using amino-propyl (NH₂) Solid Phase Extraction cartridge. The method limit of quantitation (MLOQ) was 0.01 mg/kg. The linearity of matrix-matched calibration curve (r²) was ≥0.99 at the calibration range of 0.001-0.05 mg/kg. For recovery test, Atractylodes macrocephala Koidzumi or Achyranthes japonica Nakai was treated with standard solutions at MLOQ and 10MLOQ levels. Recovery rates were in the range of 88.1-109.1% with <5.5% coefficient of variation. This established analytical method was fully validated. Based on these results, it can contribute to improving the safety of residual pesticides in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai.

• Analytical Science and Technology
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• v.19 no.3
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• pp.244-254
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• 2006

Flame retardants are added to prevent catching fire and to slow down the burning process. PBDEs are known to affect thyroid hormones and hormone disruption. The aim of this study was to propose a manual for determination of PBDEs, and investigate the accumulation of PBDEs(BDE-28, 47, 99, 100, 153, 154 and 183) in fish&shellfish and human milk samples. Pre-treatment for PBDEs determination, alkali digestion and L-L(Liquid-Liquid) extraction method could be applied to fish and shellfish. When Multi-layer column was used for cleaning up the sample, 50 mL of hexane and 100 mL of hexane:dichloromethane(9:1) solutions were used for pre- and post-elution, respectively. Activated-carbon column was optimized by a 100 mL of hexane:dichloromethane(3:1). The result of fish, highest concentration was detected in flatfish, 890 pg/g(wet weight). The other side, lowest concentration was detected in pollack, 40 pg/g(wet weight). The result of breast milk, PBDEs was detected 2,580 and 3,600 pg/g(lipid weight) from breast milk of Seoul and Juju, respectively. BDE-153 and 183 were not detected in all samples. There was no difference in PBDEs level was not difference between first and second delivery. In this study, we could find that PBDEs level in Korea is lower than other countries.

• Analytical Science and Technology
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• v.22 no.3
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• pp.219-227
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• 2009

The steroid compounds in Rhodiola sachalinensis were determined with adsorption column chromatographic purification and GC/MS. Sterols were extracted by sonication and Soxhlet with ethanol and dichloromethane, respectively. The extract was partitioned with chloroform and water using liquid-liquid extraction, and purified with a silica column after the sterols had been converted to the corresponding silyl derivatives with BSTFA. Eighteen free sterols, including $\beta$-sitosterol, stigmasterol and cycloartenol, and nine sterol conjugates were found from Rhodiola sachalinensis by GC/MS. Among them, cholest-5-ene-3-ol, cholesterol, stigmasterol, $\beta$-sitosterol were confirmed and quantified with sterol standards. Most sterols were presented in the chloroform part, with $C_{29}$ being the most abundant group in this sterol group. $\beta$-sitosterol was the most abundant compound with a relative content of 45.94% followed by ergost-7-ene-3-ol (11.33%), 4,14-dimethyl-ergosta-8,24(28)-diene-3-ol (7.07%), stigmasterol (6.09%), cycloartenol (5.43%) and 4-methyl-cholest-5-ene-3-ol (5.39%).

• Proceedings of the Korean Society of Crop Science Conference
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• 2022.10a
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• pp.114-114
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• 2022

There are 28 families and 166 species of exotic weeds on agricultural land and among these, 23 families and 80 species of exotic weeds occur on pastures. Among them, the Solidago altissima is a perennial weed belonging to the asteraceae family and it is an exotic weed that spreads to the surrounding area using methods such as high seed production, vegetative propagation using underground rhizomes and allelochemical. Accordingly, in 2009, the Ministry of Environment designated it as an ecosystem-disrupting species. This study was conducted to obtain basic data about the effects of S.altissima derived allelochemicals on forage crops. The root of S.altissima was separated, dried in the shade and then pulverized to prepare an root powder. Powder was repeatedly extracted with methanol for 3 days and concentrated under reduced pressure to obtain an root methanol extract. Dissolve the extract in distilled water, dispense it in a separate-funnel and proceed with liquid-liquid extraction by adding equal amounts of n-haxane (Hex), chloroform (CHCI₃), ethyl acetate (EtoAC), and butanol (BuOH) in order of increasing polarity. A seed-bioassay was performed using fractions for each solvent, followed by separation and purification by silica gel column chromatography. As a result of the fraction germination test for each solvent, the IC₅₀ values using the fresh weight of each fraction were 898.3 mg L^-1, 676.3 mg L^-1, 1160 mg L^-1 and 1360 mg L^-1. CA, CB, and CC fractions were obtained through primary silica gel column chromatography that used CHCI₃ fraction. As a result of seed-bioassay using each fraction, the IC₅₀ values for the fresh weight of each fraction was 537.3 mg L^-1, 1280 mg L^-1 and 1947 mg L^-1. Based on this, 5 fractions were obtained as a result of secondary silica gel column chromatography using the CA fraction. A seed-bioassay was performed, as a result, the lowest IC₅₀ value was calculated as 226.7 mg L^-1 in the CAE fraction. Based on this, the fraction was analyzed by GC-MS. The results of this study can be used as basic research data on the effects of weeds on forage crops and allelochemicals secreted from S. altissima.