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Quantification of Allantoin in Yams (Dioscorea sp.) Using a 1H NMR Spectroscopic Method

  • Thao Quyen Cao;Dongyup Hahn
    • Journal of Microbiology and Biotechnology
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    • v.33 no.5
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    • pp.662-667
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    • 2023
  • Allantoin is an abundant component of yams and has been known as a skin protectant due to its pharmacological activities. In previous methods for allantoin determination using high-performance liquid chromatography (HPLC), the separation was unsatisfactory. We herein developed a 1H quantitative nuclear magnetic resonance (qNMR) method for quantification of allantoin in the flesh and peel of yams. The method was carried out based on the relative ratio of signals integration of allantoin to a certain amount of the internal standard dimethyl sulfone (DMSO2) and validated in terms of specificity, linearity (range 62.5-2000 ㎍/ml), sensitivity (limit of detection (LOD) and quantification (LOQ) 4.63 and 14.03 ㎍/ml, respectively), precision (RSD% 0.02-0.26), and recovery (86.35-92.11%). The method was then applied for the evaluation of allantoin in flesh and peel extracts of four different yams cultivated in Korea.

A Continuous Monitoring System for the Determination of Cyanide Ions Using Nickel Complexation Reaction (흡수분광법을 적용한 시안화이온의 연속 모니터링 장치 구성 및 적용)

  • Kim, Kyung Min;Lee, Sang Hak;Kim, Young Ho;Kim, Gyu Man;Oh, Sang-Hyub
    • Applied Chemistry
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    • v.16 no.1
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    • pp.25-28
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    • 2012
  • A determination method of cyanide ion (CN-) using nickel complexation reaction by continuous monitoring system. The mechanical parameters and chemical conditions of the complexation reaction were investigated prior to application of continuous monitoring system for determination of cyanide. On the optimized conditions, the calibration curve was linear over the range from 5.0×10-6 to 1.0×10-4 M. In this range, 2.40% of the reproducibility (RSD, n=3) was obtained. The limit of detection (3σ/s) was calculated to be 1.8×10-6 M.

Development of a Simultaneous Analytical Method for Determination of Insecticide Broflanilide and Its Metabolite Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살충제 Broflanilide 및 대사물질 동시시험법 개발)

  • Park, Ji-Su;Do, Jung-Ah;Lee, Han Sol;Park, Shin-min;Cho, Sung Min;Kim, Ji-Young;Shin, Hye-Sun;Jang, Dong Eun;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.124-134
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    • 2019
  • An analytical method was developed for the determination of broflanilide and its metabolites in agricultural products. Sample preparation was conducted using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and LC-MS/MS (liquid chromatograph-tandem mass spectrometer). The analytes were extracted with acetonitrile and cleaned up using d-SPE (dispersive solid phase extraction) sorbents such as anhydrous magnesium sulfate, primary secondary amine (PSA) and octadecyl ($C_{18}$). The limit of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The recovery results for broflanilide, DM-8007 and S(PFP-OH)-8007 ranged between 90.7 to 113.7%, 88.2 to 109.7% and 79.8 to 97.8% at different concentration levels (LOQ, 10LOQ, 50LOQ) with relative standard deviation (RSD) less than 8.8%. The inter-laboratory study recovery results for broflanilide and DM-8007 and S (PFP-OH)-8007 ranged between 86.3 to 109.1%, 87.8 to 109.7% and 78.8 to 102.1%, and RSD values were also below 21%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food and Drug Safety Evaluation guidelines (2016). Therefore, the proposed analytical method was accurate, effective and sensitive for broflanilide determination in agricultural commodities.

Simultaneous Analysis for Veterinary Drug Residues in Honey by HPLC/MS/MS (HPLC-MS/MS를 이용한 벌꿀 중 동물용의약품 동시분석방법 연구)

  • Kim, Jong-Hwa;Moon, Sun-Ea;Kim, Ki-Yu;Jung, You-Jung;Lee, Chang-Hee;Ku, Eun-Jung;Yoon, Mi-Hye;Lee, Jong-Bok
    • Journal of Food Hygiene and Safety
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    • v.31 no.2
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    • pp.94-98
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    • 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.

Immunocytochemical Localization of Parvalbumin and Calbindin-D 28K in Monkey Dorsal Lateral Geniculate Nucleus (원숭이 외측슬상체배측핵에서 칼슘결합단백 Parvalbumin과 Calbindin-D 28K의 분포)

  • Ko, Seung-Hee;Bae, Choon-Sang;Park, Sung-Sik
    • Applied Microscopy
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    • v.24 no.4
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    • pp.61-77
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    • 1994
  • The calcium-binding proteins (CaBP), parvalbumin (PV) and calbindin-D 28K (calbindin) are particularly abundant and specific in their distribution, and present in different subsets of neurons in many brain regions. Although their physiological roles in the neurons have not been elucidated, they are valuable markers of neuronal subpopulations for anatomical and developmental studies. This study is designed to characterize dorsal lateral geniculate nucleus (dLGN) neurons and axon terminals in terms of differential expression of immunoreactivity (IR) for two well-known CaBPs, PV and calbindin. The experiments were carried out on 6 adult monkeys. Monkeys were perfused under deep Nembutal anesthesia with 2% paraformaldehyde and 0.2% glutaraldehyde in 0.1M phosphate buffer. After removal, the brains were postfixed for 6-8 hr in 2% paraformaldehyde at $4^{\circ}C$ and infiltrated with 30% sucrose at $4^{\circ}C$. Thereafter, they were frozen in dry ice. Serial sections of the thalamus, at $20{\mu}m$, were made in the frontal plane with a sliding microtome. The sections were stained for PV and calbindin with indirect immunocytochemical methods. For electron microscopy, after infiltration with 30% sucrose the blocks of thalamus were serially sectioned at $50{\mu}m$ with a Vibratome in the coronal plane and stained immediately by indirect ABC methods without Triton X-100 in incubation medium. Stained sections were postfixed in 0.2% osmium tetroxide, dehydrated and flat-embedded in Spurr resin. The block was then trimmed to contain only a selected lamina or interlaminar space. The dLGN proper showed strong PV IR in fibers in all laminae and interlaminar zones. Particularly dense staining was noted in layers 1 and 2 that contain many stained fibers from optic tract. Neuronal cell body stained with PV was concentrated only in the laminae. In these laminae staining was moderate in cell bodies of all large and medium-sized neurons, and was strong in cell bodies of some small neurons together with their processes. Calbindin IR was marked in the neuronal cell body and neuropil in the S layers and interlaminar zones whereas moderate in the neuropil throughout the nucleus. Regional difference in distribution of PV and calbindin IR cell is distinct; the former is only in the laminae and the latter in both the S layer and interlaminar space. The CaBP-IR elements were confined to about $10{\mu}m$ in depth of Vibratome section. The IR product for CaBP was mainly associated with synaptic vesicle, pre- and post-synaptic membrane, and outer mitochondrial membrane and along microtubule. PV-IR was noted in various neuronal elements such as neuronal soma, dendrite, RLP, F, PSD and some myelinated or unmyelinated axons, and was not seen in the RSD and glial cells. Only a few neuronal components in dLGN was IR for calbindin and its reaction product was less dense than that of PV, and scattered throughout cytoplasm of soma of some relay neurons, and was also persent in some dendrite, myelinated axons and RLP. The RSD, F, PSD and glial elements were always non-IR for calbindin. Calbindin labelled RLP were presynaptic to unlabeled dendrite or dendritic spine and PSD. Calbindin-labeled dendrite of various sizes were always postsynaptic to unlabeled RSD, RLP or F. From this study it is suggested that dLGN cells of different functional systems and their differential projection to the visual cortex can be distinguished by differential expression of PV and calbindin.

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Species Diversity Analysis of the Mushroom in Mt. Chiak (치악산 발생 버섯의 종 다양성 비교 분석)

  • Lee, Byung Kook;Eom, Ki Cheol;Seok, Soon Ja
    • The Korean Journal of Mycology
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    • v.41 no.2
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    • pp.57-66
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    • 2013
  • The mushrooms collected at seven areas of Mt. Chiak in 2002 and 2003 were classified to analyse the distribution and species diversity. Frequency (number of mushroom : N), number of species (S), relative species density (RSD), similarity index (C), richness index (R1), variety index (V1), evenness index (E2), and dominance index(D1) were investigated. Total N and S was 143 and 84, respectively. The RSD was 0.179 ~ 0.226 of the 7 areas. The yearly C of the total area (0.213) was 8.2%. more higher than the average C of 7 areas (0.131). The order in the coefficient of variation (CV) of the indicator for 7 areas was N (10.5%) > D1 (9.2%) > V1 (8.9%) > S (8.5%) > R1 (7.4%) > E2 (2.2%). The average R1 of the 7 areas was 5.36 with the range from 4.85 to 6.01, and 16.72 for the total area. The average V1 of the 7 areas was 16.24 with the range from 14.44 to 18.66, and 68.82 for the total area. The average E2 of the 7 areas was 0.95 with the range from 0.926 to 0.982, and 0.819 for the total area. The average D1 of the 7 areas was 0.071 with the range from 0.055 to 0.073, and 0.081 for the total area. The correlation between N and 5 kinds of diversity indicator (S, R1, V1, E2, D) was not statistically significant, but the correlation between R1, E2 and D1 was statistically significant each other.

Development and Validation of Analytical Method for Determination of Biphenyl Analysis in Foods (식품 중 비페닐 분석법 개발 및 유효성 검증)

  • Kim, Jung-Bok;Kim, Myung-Chul;Song, Sung-Woan;Shin, Jae-Wook
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.4
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    • pp.459-464
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    • 2017
  • Biphenyl is used as an intermediate in the production of crop protection products, a solvent in pharmaceutical production, and as a component in the preservation of citrus fruits in many countries. Biphenyl is not authorized for use and also does not have standards or specifications as a food additive in Korea. National and imported food products are likely to contain biphenyl. Therefore, control and management of these products is required. In this study, a simple analytical method was developed and validated using HPLC to determine biphenyl in food. These methods are validated by assessing certain performance parameters: linearity, accuracy, precision, recovery, limit of detection (LOD), and limit of quantitation (LOQ). The calibration curve was obtained from 1.0 to $100.0{\mu}g/mL$ with satisfactory relative standard deviations (RSD) of 0.999 in the representative sample (orange). In the measurement of quality control (QC) samples, accuracy was in the range of 95.8~104.0% within normal values. The inter-day and inter-day precision values were less than 2.4% RSD in the measurement of QC samples. Recoveries of biphenyl from spiked orange samples ranged from 92.7 to 99.4% with RSD between 0.7 and 1.7% at levels of 10, 50, and $100{\mu}g/mL$. The LOD and LOQ were determined to be 0.04 and $0.13{\mu}g/mL$, respectively. These results show that the developed method is appropriate for biphenyl identification and can be used to examine the safety of citrus fruits and surface treatments containing biphenyl residues.

Evaluation of confidence for measurement of VOCs in indoor air (실내공기질 VOCs 측정의 신뢰도 평가를 위한 연구)

  • Kim, Myoung Ock;Kim, Young Lan;Hong, Suk Young;Heo, Gwi Suk;Lim, Hyun Woo;Choe, Seoung Hun;Lee, Won Suk;Han, Jin Seok;Kim, Kum Hee
    • Analytical Science and Technology
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    • v.26 no.3
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    • pp.165-173
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    • 2013
  • To establishment of PT Program for Indoor air quality field that manufacture of confidential development PTMs (proficiency testing materials) and examined of proficiency testing evaluation included sampling process whether or not that is valid. Confirmation of homogeneity and stability of PTMs prepared. PTMs were confirmed to be homogeneous enough to be used as proficiency testing materials since withinbottle homogeneities of the RMs were lower than 0.3 times of targeted standard deviation of proficiency testing. The result of this study showed that the Robust RSD of proficiency testing for VOCs (volatile organic compounds) appeared 23~43% in concentration of 50~320 ${\mu}g/m^3$ for Method A(Distribution by adsorption in Tenax-tube of VOCs), but less 13~42% in concentration of 200~1200 ${\mu}g/m^3$, 16~31% in concentration of 100~450 ${\mu}g/m^3$ for Method B (distribution by VOCs of gas phase in 10L Tedalr bag), C (directly sampling of cylinder with high pressure) respectively. The result of this study showed that method C with sampling is most adequate to the proficiency testing for VOCs in indoor air.

Analysis of Hydrodynamics in a Directly-Irradiated Fluidized Bed Solar Receiver Using CPFD Simulation (CPFD를 이용한 태양열 유동층 흡열기의 수력학적 특성 해석)

  • Kim, Suyoung;Won, Geunhye;Lee, Min Ji;Kim, Sung Won
    • Korean Chemical Engineering Research
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    • v.60 no.4
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    • pp.535-543
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    • 2022
  • A CPFD (Computational particle fluid dynamics) model of solar fluidized bed receiver of silicon carbide (SiC: average dp=123 ㎛) particles was established, and the model was verified by comparing the simulation and experimental results to analyze the effect of particle behavior on the performance of the receiver. The relationship between the heat-absorbing performance and the particles behavior in the receiver was analyzed by simulating their behavior near bed surface, which is difficult to access experimentally. The CPFD simulation results showed good agreement with the experimental values on the solids holdup and its standard deviation under experimental condition in bed and freeboard regions. The local solid holdups near the bed surface, where particles primarily absorb solar heat energy and transfer it to the inside of the bed, showed a non-uniform distribution with a relatively low value at the center related with the bubble behavior in the bed. The local solid holdup increased the axial and radial non-uniformity in the freeboard region with the gas velocity, which explains well that the increase in the RSD (Relative standard deviation) of pressure drop across the freeboard region is responsible for the loss of solar energy reflected by the entrained particles in the particle receiver. The simulation results of local gas and particle velocities with gas velocity confirmed that the local particle behavior in the fluidized bed are closely related to the bubble behavior characterized by the properties of the Geldart B particles. The temperature difference of the fluidizing gas passing through the receiver per irradiance (∆T/IDNI) was highly correlated with the RSD of the pressure drop across the bed surface and the freeboard regions. The CPFD simulation results can be used to improve the performance of the particle receiver through local particle behavior analysis.

Development of a Simultaneous Analysis Method for Disapproved Coloring Agents in Foods Using HPLC (HPLC를 이용한 식품중 허용 외 색소의 동시분석에 관한 연구)

  • Kim, Cheon-Hoe;Lee, Min-Jae;Kim, Keoung-Ok;Lee, Hyoun-Young;Yang, Joo-Hong;Heo, Seok;Park, Jong-Seok;Jang, Yeong-Mi;Kim, Hee-Yun
    • Korean Journal of Food Science and Technology
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    • v.40 no.4
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    • pp.375-381
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    • 2008
  • This study developed the simultaneous analysis method for efficient safety controls of import food of Orange II, Rhodamine B, Para Red, and Sudan dye I-IV among disapproved coloring agents that use is prohibited in foods. The analysis method was developed according to the sample pre-treatment and HPLC conditions, and a documentary survey was used to establish the detection limit of the method, followed by effectiveness verification and recovery percentage examinations. Recovery percentage examination for 26 products resulted Orange II displayed recovery percentage of 96.46-121.26%, Rhodamine B displayed recovery percentage of 70.86-106.53%, Para Red displayed recovery percentage of 97.00-116.86%, Sudan I displayed recovery percentage of 92.93-112.44%, Sudan II displayed recovery percentage of 96.63-115.10%, Sudan III displayed recovery percentage of 92.21-114.73%, Sudan IV displayed recovery percentage of 93.22-122.91%. Correlation coefficient of gradient of this analysis method exhibited more than 0.999, RSD exhibited fewer than 2 as 0.8-1.39%, exactitude exhibited more than 90%. At this time, detection limit and fixed quantity limit decided by each 0.1 mg/L, 0.3 mg/L.