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Determination of Flunixin and 5-Hydroxy Flunixin Residues in Livestock and Fishery Products Using Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS)

  • Dahae Park;Yong Seok Choi;Ji-Young Kim;Jang-Duck Choi;Gui-Im Moon
    • Food Science of Animal Resources
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    • v.44 no.4
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    • pp.873-884
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    • 2024
  • Flunixin is a veterinary nonsteroidal anti-inflammatory agent whose residues have been investigated in their original form within tissues such as muscle and liver. However, flunixin remains in milk as a metabolite, and 5-hydroxy flunixin has been used as the primary marker for its surveillance. This study aimed to develop a quantitative method for detecting flunixin and 5-hydroxy flunixin in milk and to strengthen the monitoring system by applying to other livestock and fishery products. Two different methods were compared, and the target compounds were extracted from milk using an organic solvent, purified with C18, concentrated, and reconstituted using a methanol-based solvent. Following filtering, the final sample was analyzed using liquid chromatography-tandem mass spectrometry. Method 1 is environmentally friendly due to the low use of reagents and is based on a multi-residue, multi-class analysis method approved by the Ministry of Food and Drug Safety. The accuracy and precision of both methods were 84.6%-115% and 0.7%-9.3%, respectively. Owing to the low matrix effect in milk and its convenience, Method 1 was evaluated for other matrices (beef, chicken, egg, flatfish, and shrimp) and its recovery and coefficient of variation are sufficient according to the Codex criteria (CAC/GL 71-2009). The limits of detection and quantification were 2-8 and 5-27 ㎍/kg for flunixin and 2-10 and 6-33 ㎍/kg for 5-hydroxy flunixin, respectively. This study can be used as a monitoring method for a positive list system that regulates veterinary drug residues for all livestock and fisheries products.

A Multidimensional System for Phosphopeptide Analysis Using TiO2 Enrichment and Ion-exchange Chromatography with Mass Spectrometry

  • Cho, Kun;Yoo, Ji-Sun;Kim, Eun-Min;Kim, Jin-Young;Kim, Young-Hwan;Oh, Han-Bin;Yoo, Jong-Shin
    • Bulletin of the Korean Chemical Society
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    • v.33 no.10
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    • pp.3298-3302
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    • 2012
  • Although offline enrichment of phosphorylated peptides is widely used, enrichment for phosphopeptides using $TiO_2$ is often performed manually, which is labor-intensive and can lead to irreproducible results. To address the problems associated with offline enrichment and to improve the effectiveness of phosphopeptide detection, we developed an automated online enrichment system for phosphopeptide analysis. A standard protein mixture comprising BSA, fetuin, crystalline, ${\alpha}$-casein and ${\beta}$-casein, and ovalbumin was assessed using our new system. Our multidimensional system has four main parts: a sample pump, a 20-mm $TiO_2$-based column, a weak anion-exchange, and a strong cation-exchange (2:1 WAX:SCX) separation column with LC/MS. Phosphorylated peptides were successfully detected using the $TiO_2$-based online system with little interference from nonphosphorylated peptides. Our results confirmed that our online enrichment system is a simple and efficient method for detecting phosphorylated peptides.

Enhanced Photosensitivity in Monolayer MoS2 with PbS Quantum Dots

  • Cho, Sangeun;Jo, Yongcheol;Woo, Hyeonseok;Kim, Jongmin;Kwak, Jungwon;Kim, Hyungsang;Im, Hyunsik
    • Applied Science and Convergence Technology
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    • v.26 no.3
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    • pp.47-49
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    • 2017
  • Photocurrent enhancement has been investigated in monolayer (1L) $MoS_2$ with PbS quantum dots (QDs). A metal-semiconductor-metal (Au-1L $MoS_2$-Au) junction device is fabricated using a standard photolithography method. Considerably improved photo-electrical properties are obtained by coating PbS QDs on the Au-1L $MoS_2$-Au device. Time dependent photoconductivity and current-voltage characteristics are investigated. For the QDs-coated $MoS_2$ device, it is observed that the photocurrent is considerably enhanced and the decay life time becomes longer. We propose that carriers in QDs are excited and transferred to the $MoS_2$ channel under light illumination, improving the photocurrent of the 1L $MoS_2$ channel. Our experimental findings suggest that two-dimensional layered semiconductor materials combined with QDs could be used as building blocks for highly-sensitive optoelectronic detectors including radiation sensors.

Production of a New Biosurfactant by a New Yeast Species Isolated from Prunus mume Sieb. et Zucc.

  • Jeong-Seon Kim;Miran Lee;Dae-Won Ki;Soon-Wo Kwon;Young-Joon Ko;Jong-Shik Kim;Bong-Sik Yun;Soo-Jin Kim
    • Journal of Microbiology and Biotechnology
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    • v.33 no.8
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    • pp.1023-1029
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    • 2023
  • Biosurfactants reduce surface and interfacial tension due to their amphiphilic properties and are an eco-friendly alternative for chemical surfactants. In this study, a new yeast strain JAF-11 that produces a biosurfactant was selected using drop collapse method, and the properties of the extracts were investigated. The nucleotide sequences of the strain were compared with closely related strains and identified based on the D1/D2 domain of the large subunit ribosomal DNA (LSU) and internal transcribed spacer (ITS) regions. Neodothiora populina CPC 39399T, the closest species with strain JAF-11, showed a sequence similarity of 97.75% for LSU and 94.27% for ITS, respectively. The result suggests that the strain JAF-11 represents a distinct species that cannot be assigned to any existing genus or species in the family Dothideaceae. Strain JAF-11 produced a biosurfactant reducing the surface tension of water from 72 mN/m to 34.5 mN/m on the sixth day of culture and the result of measuring the critical micelle concentration (CMC) by extracting the crude biosurfactant was found to be 24 mg/l. The molecular weight 502 of the purified biosurfactant was confirmed by measuring the fast atom bombardment mass spectrum. The chemical structure was analyzed by measuring 1H nuclear magnetic resonance (NMR), 13C NMR, and two-dimensional NMRs of the compound. The molecular formula was C26H46O9, and it was composed of one octanoyl group and two hexanoyl groups to myo-inositol moiety. The new biosurfactant is the first report of a compound produced by a new yeast strain, JAF-11.

Comparison of QuEChERS and Solid Phase Extraction for Accurate Determination of Pesticide Residues in Kimchi Cabbage and Strawberry using Isotope Dilution Mass Spectrometry

  • Seonghee Ahn;Kebede Gebeyehu Mekete;Byungjoo Kim
    • Mass Spectrometry Letters
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    • v.14 no.4
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    • pp.178-185
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    • 2023
  • QuEChERS is used worldwide as a universal sample preparation method with many benefits, such as being quick, easy, cheap, effective, rugged and safe. This study examined whether QuEChERS can be employed in isotope dilution mass spectrometry (ID-MS) for accurate analysis of pesticides in food. The ratios of fortified values and measured values of malathion and fenitrothion using the QuEChERS method were compared with those using the solid phase extract (SPE) method which was previously used in this laboratory. The separations of the two pesticides on DB-5MS and VF-1701MS columns were compared. Malathion and fenitrothion were fortified into kimchi cabbage and pretreated with the QuEChERS method and the SPE method. The results obtained using the DB-5MS column varied according to the sample preparation method, column and pesticide level. Using the VF-1701 column, ratios were 98-102% by both QuEChERS and Carb/NH2 SPE method for all fortification level. Malathion and fenitrothion were fortified into strawberry samples for comparison with kimchi cabbage. The results for the strawberry samples indicated that the ratios were not influenced by the sample preparation methods or GC column. The QuEChERS method could be acceptable in the ID-MS method for pesticide residue analysis in food, however other conditions should be carefully considered for accurate determination, such as the column, amount of analyte and food matrix.

A Real Scale Experimental Study for Evaluation of Permissible Shear Stresses on Vegetation Mats (식생매트 허용 소류력 평가를 위한 실규모 실험 연구)

  • Lee, Du Han;Kim, Dong-Hee;Kim, Myounghwan;Rhee, Dong Sop
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.13 no.12
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    • pp.6151-6158
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    • 2012
  • By the activation of environment-friendly river works, application of vegetation mats is increasing, however, evaluation techniques for hydraulic stability of vegetation mats are not presented. This study is conducted to develop the objective test method for vegetation mats. Two kind of vegetation mats are tested by the real scale experiments, and hydraulic quantities are measured and analyzed to evaluate acting shear stresses. Roughness and shear stress are evaluated by 1 D non-uniform model. After each tests, changes in mat surfaces and sub-soil are evaluated, and from these evaluation, 3 types of mat surface damages and 2 types of sub-soil damages are presented. In the study, the case in which some damages in mat surface don't cause loss of sub-soil, is presented to be in the stable condition. Appling this stable condition and acting shear stresses, permissible shear stresses of vegetation mats are evaluated, and the results show that the reinforced mat with wire netting has more permissible shear stress.

MoS2/CNFs derived from Electrospinning and Heat treatment as the Efficient Electrocatalyst for Hydrogen Eovlution Reaction in Acidic Solution (전기 방사를 이용한 1D / 2D 하이브리드 구조 고활성 MoS2 / CNF 수소 발생 촉매의 합성 및 특성 분석)

  • Lee, Jeong Hun;Park, Yoo Sei;Jang, Myeong Je;Park, Sung Min;Lee, Kyu Hwan;Choi, Woo Sung;Choi, Sung Mook;Kim, Yang Do
    • Korean Journal of Metals and Materials
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    • v.56 no.12
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    • pp.885-892
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    • 2018
  • Molybdenum disulfide ($MoS_2$) based electrocatalysts have been proposed as substitutes for platinum group metal (PGM) based electrocatalyst to hydrogen evolution reaction (HER) in water electrolysis. Here, we studied $MoS_2/CNFs$ hybrid catalyst prepared by electrospinning method with heat treatment for polymer electrolyte membrane(PEM) water electrolysis to improve the HER activity. The physicochemical and electrochemical properties such as average diameter, crystalline properties, electrocatalitic activity for HER of synthesized $MoS_2/CNFs$ were investigated by the Scanning Electron Microscope (SEM), X-ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Transmission Electron Microscopy (TEM), Raman Spectroscopy (Raman) and Linear Sweep Voltammetry (LSV). The as spun ATTM/PVP nanofibers were prepared by sol-gel and electrospinning method. Subsequently, the $MoS_2/CNFs$ was dereived from reduction heat treatment of ATTM at the ATTM/PVP nanofibers and carbonization heat treatment. Synthesized $MoS_2/CNFs$ electrocatalyst had an average diameter of $179{\pm}30nm$. We confirmed that the $MoS_2$ layers in $MoS_2/CNF$ electrocatalyst consist of 3~4 layers from the Raman results. In addition, We confirmed that the $MoS_2$ layers in $MoS_2/CNF$ catalyst consist of 7.47% octahedral 1T phase $MoS_2$, 63.77% trigonal prismatic 2H phase $MoS_2$ with 28.75% $MoO_3$ through the XRD, Raman and XPS results. It was shown that $MoS_2/CNFs$ had the overpotential of 0.278 V at $10mA/cm^2$ and tafel slope of 74.8 mV/dec in 0.5 M sulfuric acid ($H_2SO_4$) electrolyte.

Enhanced Production of C30 Carotenoid 4,4'-Diaponeurosporene by Optimizing Culture Conditions of Lactiplantibacillus plantarum subsp. plantarum KCCP11226T

  • Siziya, Inonge Noni;Yoon, Deok Jun;Kim, Mibang;Seo, Myung-Ji
    • Journal of Microbiology and Biotechnology
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    • v.32 no.7
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    • pp.892-901
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    • 2022
  • The rising demand for carotenoids can be met by microbial biosynthesis as a promising alternative to chemical synthesis and plant extraction. Several species of lactic acid bacteria (LAB) specifically produce C30 carotenoids and offer the added probiotic benefit of improved gut health and protection against chronic conditions. In this study, the recently characterized Lactiplantibacillus plantarum subsp. plantarum KCCP11226T produced the rare C30 carotenoid, 4,4'-diaponeurosporene, and its yield was optimized for industrial production. The one-factor-at-a-time (OFAT) method was used to screen carbon and nitrogen sources, while the abiotic stresses of temperature, pH, and salinity, were evaluated for their effects on 4,4'-diaponeurosporene production. Lactose and beef extract were ideal for optimal carotenoid production at 25℃ incubation in pH 7.0 medium with no salt. The main factors influencing 4,4'-diaponeurosporene yields, namely lactose level, beef extract concentration and initial pH, were enhanced using the Box-Behnken design under response surface methodology (RSM). Compared to commercial MRS medium, there was a 3.3-fold increase in carotenoid production in the optimized conditions of 15% lactose, 8.3% beef extract and initial pH of 6.9, producing a 4,4'-diaponeurosporene concentration of 0.033 A470/ml. To substantiate upscaling for industrial application, the optimal aeration rate in a 5 L fermentor was 0.3 vvm. This resulted in a further 3.8-fold increase in 4,4'-diaponeurosporene production, with a concentration of 0.042 A470/ml, compared to the flask-scale cultivation in commercial MRS medium. The present work confirms the optimization and scale-up feasibility of enhanced 4,4'-diaponeurosporene production by L. plantarum subsp. plantarum KCCP11226T.

Study for Residue Analysis of Pinoxaden in Agricultural Commodities

  • Kim, Ji Young;Yoon, Eun Kyung;Kim, Jong Soo;Seong, Nu Ri;Yun, Sang Soon;Jung, Yong Hyun;Oh, Jae Ho;Kim, Hyochin
    • Korean Journal of Environmental Agriculture
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    • v.38 no.4
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    • pp.321-331
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    • 2019
  • BACKGROUND: Pinoxaden is the phenylpyrazoline herbicide developed by Syngenta Crop Protection, Inc. and marketed on 2006. The maximum residue levels for wheat and barley were set by import tolerance. Thus, Ministry of Food and Drug Safety (MFDS) official analytical method determining Pinoxaden residue was necessary in various food matrixes. Satisfaction of international guideline of CODEX (Codex Alimentarius Commission CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) are additional pre-requirements for analytical method. In this study, liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was investigated to analyze residue of Pinoxaden (M4), which is defined as pesticide residue in Korea, in foods. METHODS AND RESULTS: Pinoxaden (M4) was extracted followed by acid digestion (2hr reflux with 1N HCl) and pH adjusting (pH 4-5 with 3% ammonium solution). To remove oil, additional clean-up step with hexane saturated with acetonitrile was required to high oil contained sample before purification. HLB cartridge and nylon syringe filter were used for purification. Then, samples were analyzed by LC-MS/MS using reserve phase column C18. Five agricultural group representative commodities (mandarin, potato, soybean, hulled rice, and red pepper) were used to verify the method in this study. The liner matrix-matched calibration curves were confirmed with coefficient of determination (r2) > 0.99 at calibration range 0.002-0.2 mg/kg. The limits of detection and quantitation were 0.004 and 0.01 mg/kg, respectively, which were suitable to apply Positive List System (PLS). Mean average accuracies of pinoxaden (M4) were shown to be 74.0-105.7%. The precision of pinoxaden and its metabolites were also shown less than 14.5% for all five samples. CONCLUSION: The method investigated in this study was suitable to CODEX (CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

Multi-Residue Analysis of 18 Dye Residues in Animal Products by Liquid Chromatography-Tandem Mass Spectrometry

  • Park, Hyunjin;Kim, Joohye;Kang, Hui-Seung;Cho, Byung-Hoon;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.35 no.2
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    • pp.109-117
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    • 2020
  • This study aimed to develop an analytical method for determination of 18 dyes in livestock and fishery products by liquid chromatograph-tandem mass spectrometry (LC-MS/MS). The developed method was validated for linearity, accuracy, limit of quantifications (LOQ) and recovery based on the CODEX guideline (CAC/GL-71). Target matrices (beef, pork, chicken, egg, milk, flatfish, eel, and shrimp) were extracted using acetonitrile (containing 1% of acetic acid) and then, purified with C18 and primary secondary amine (PSA). Calibration linearity was obtained (r2>0.98) and LOQs were 0.002 mg/kg in animal products. The recoveries of dyes were ranged from 63 to 112% and relative standard deviations (RSDs, %) were less than 15%. The residues of 18 dyes were investigated in real samples (n=124) collected from retail markets in South Korea. As a result, a total of seven samples showed positive results for target analytes in fish samples. However, there was no violation according to the maximum residue limits set by the Korean Food Code. The proposed method will be used for routine analysis of dye residues in livestock and fishery products.