• Title/Summary/Keyword: phase detection

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Simultaneous determination of preservatives in sausages using liquid chromatography with electrospray ionization tandem mass spectrometry (LC-MS/MS를 이용한 소시지 중 보존료 동시분석)

  • Koh, Ba-Ra-Da;Kim, Ji-Yeon;Jang, Mi-Sun;Seo, Doo-Ri;Jung, Bo-Ram;Shin, Ji-Hyun;Lim, Jin-Taek;Kim, Yong-Hwan;Kim, Eun-Sun
    • Korean Journal of Veterinary Service
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    • v.38 no.2
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    • pp.127-136
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    • 2015
  • A simultaneous determination method was developed for nine preservatives (benzoic acid, sorbic acid, dehydroacetic acid, methyl-, ethyl-, isopropyl-, propyl-, isobutyl- and butyl-parabens) in sausage by liquid chromatography with electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS). Each parameter was established by multiple reaction monitoring in negative mode. Separation was achieved on a phenyl-hexyl ($2.5{\mu}m$, $2.1{\times}150mm$, Waters) with A-20 mM ammonium acetate containing 0.1% acetic acid in water, B-Acetonitrile as mobile phase with gradient mode at a flow rate of 0.3 mL/min. The developed method was validated for specificity, linearity, accuracy and precision in sausages samples. Linearity was over 0.998 with calibration curve of the mixed standards. The mean recoveries from sausages fortified at the level of 2.0~10.0 mg/L were in range of 98.60~109.16% with RSDs lower than 8.93%. The limits of detection (LOD) and the limits of quantification (LOQ) were in the range between 0.0003~0.085 mg/L and 0.01~0.257 mg/L, respectively. Intra-day precision and inter-day precision were 0.45~6.16% and 2.81~13.33%, respectively. Using presently developed determination method, 33 field sausage samples from Gwangju city in Korea were screened over nine preservatives. As a result, no preservatives were detected in all samples.

Analysis of Vitamin K1 in Commonly Consumed Foods in Korea (국내에서 소비되는 상용 식품의 비타민 K1 함량 분석)

  • Lee, Seongeung;Sung, Jeehye;Choi, Youngmin;Kim, Youngwha;Jeong, Heon-Sang;Lee, Junsoo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.8
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    • pp.1194-1199
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    • 2015
  • Vitamin $K_1$ (phylloquinone) content of commonly consumed foods in Korea were determined by solvent extraction followed by reversed-phase liquid chromatography using post-column derivatization and fluorescence detection. Samples were obtained in the years of 2013 and 2015. In this study, 46 vegetables, 14 fruits, and 6 legumes were analyzed. Relatively higher amounts of vitamin $K_1$ were found in sweet potato leaves, green kiwi, and mung beans among vegetables, fruits, and legumes, respectively. The content of vitamin $K_1$ in vegetables including spinach, broccoli, and potato ranged from non-detectable (ND) to $1,467.3{\mu}g/100g$. The content of vitamin $K_1$ in fruits ranged from ND to $42.7{\mu}g/100g$. The content of vitamin $K_1$ in legumes, including soybeans, mung beans and peas ranged from 1.7 to $63.4{\mu}g/100g$. In addition, the analytical method validation parameters including recovery, reproducibility, repeatability, peak purity, and linearity were calculated to ensure the method's validity. The results showed high linearity with a correlation coefficient of 0.9999. Overall recovery was close to 100% (n=5). This study revealed reliable vitamin K content in commonly consumed foods in Korea for a nutritional information and food composition database.

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.

Model Proposal for Detection Method of Cyber Attack using SIEM (SIEM을 이용한 침해사고 탐지방법 모델 제안)

  • Um, Jin-Guk;Kwon, Hun-Yeong
    • The Journal of the Institute of Internet, Broadcasting and Communication
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    • v.16 no.6
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    • pp.43-54
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    • 2016
  • The occurrence of cyber crime is on the rise every year, and the security control center, which should play a crucial role in monitoring and early response against the cyber attacks targeting various information systems, its importance has increased accordingly. Every endeavors to prevent cyber attacks is being attempted by information security personnel of government and financial sector's security control center, threat response Center, cyber terror response center, Cert Team, SOC(Security Operator Center) and else. The ordinary method to monitor cyber attacks consists of utilizing the security system or the network security device. It is anticipated, however, to be insufficient since this is simply one dimensional way of monitoring them based on signatures. There has been considerable improvement of the security control system and researchers also have conducted a number of studies on monitoring methods to prevent threats to security. In accordance with the environment changes from ESM to SIEM, the security control system is able to be provided with more input data as well as generate the correlation analysis which integrates the processed data, by extraction and parsing, into the potential scenarios of attack or threat. This article shows case studies how to detect the threat to security in effective ways, from the initial phase of the security control system to current SIEM circumstances. Furthermore, scenarios based security control systems rather than simple monitoring is introduced, and finally methods of producing the correlation analysis and its verification methods are presented. It is expected that this result contributes to the development of cyber attack monitoring system in other security centers.

Simultaneous determination of illegal galactagogue adulterants in supplement diets by LC-MS/MS

  • Lee, Ji Hyun;Cho, So-Hyun;Park, Han Na;Park, Hyoung Joon;Kim, Nam Sook;Park, Sung Kwan;Kang, Hoil
    • Analytical Science and Technology
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    • v.31 no.4
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    • pp.171-178
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    • 2018
  • Recently, for successful lactation, many breastfeeding mothers seek various products, including herbal medicine, dietary supplements, and prescribed medicines, to improve milk production. As demand for galactogogues grows, it is highly possible that pharmaceutical galactogogues may be adulterated with illegal products to maximize their efficacy. For continuous control and supervision of illegal products, we developed and validated a simple and sensitive LC-MS/MS method capable of simultaneously determining five galactogogues. Chromatographic separation was conducted using an Agilent Poroshell $120SB-C_{18}$ column with a mobile phase consisting of 20 mM ammonium formate (pH 5.4) and 100 % acetonitrile. The total run time was 13 min per analyte. The proposed method was performed according to the guidelines of the International Conference of Harmonization and it produced reliable results. This method showed high sensitivity and specificity, with a limit of detection (LOD) and limit of quantitation (LOQ) of 0.01-0.82 ng/mL and 0.02-2.45 ng/mL, respectively, for the solid- and liquid-type samples. Specificity was evaluated by analyzing matrix-blank samples spiked with the target compounds at LOQ levels, which provided a good separation of all peaks without interference. Additionally, the repeatability and intermediate precision were typically <15 %, whereas the recovery was 80-120 % of the values obtained using blank samples. Thus, we concluded that this method could be used for the identification and quantification of galactogogues in food or herbal products.

Effects and Behaviors of Heavy Metals(Cd, Cr, Cu, Pb) in Cement Clinker Reaction (시멘트 클린커 반응에서 중금속(Cd, Cr, Cu, Pb)의 거동과 영향)

  • Hong, Seong-Su;Lee, Taeck-Hong;Lim, Gye-Gyu;Oh, Hea-Kab;Lee, Bong-Han
    • Applied Chemistry for Engineering
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    • v.10 no.5
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    • pp.696-700
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    • 1999
  • The effects and behaviors of heavy metals incoming from industrial by-products were investigated in cement clinker reaction. The raw meal containing 500 ppm of heavy metal ion such as Cu, Cd, Cr, and Pb was calcined at $1450^{\circ}C$ for 30 minutes. Burnability index, fixation concentration of heavy metals in clinker, and apportionment ratio were analyzed. Pb had a minimum fixation concentration of under 5% and Cr had a maximum over 85%. The burnability of Cr containing clinker was lower than that of others as the result of higher value of 3.41% of free lime after calcination at $1450^{\circ}C$. Cu, Cd, and Pb had not any significant effects on the clinker reactitivity. The volatility of heavy metals produced lots of macropores and micropores in clinker and minerals. Cd and Cr were the major apportionments in alite and belite and Cu in interstitial phase. Pb was existed under the detection limit of EDAX analysis due to its higher volatility.

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Design and Implementation of Microstrip Quadrature Coupler and High Power Transmitting/Receiving Switch Using Dynamic Loading Technique for 1-Tesal MRI System (동적 부하 기술을 이용한 1-Tesla 자기공명 영상 시스템용 마이크로 스트립 quadrature coupler 및 고출력 송수신 스위치의 설계 및 제작)

  • 류웅환;이미영;이흥규;이황수;김정호
    • Journal of the Korean Institute of Telematics and Electronics D
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    • v.36D no.3
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    • pp.1-11
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    • 1999
  • It is now common practice to utilize the quadrature RF coils to improve the signal-to-noise ratio (SNR) in the Magnetic Resonance Imaging (MRI) System. In addition, to make such an available SNR improvement, it is mandatory to use a well-designed quadrature coupler, which facilitates a perfect 3-dB coupling and quadrature-phase shift. However, the four ports matching condition has to be well considered during the RF excitation and the signal detection period. This work investigates the effects of such a mismatching condition (especially, due to patient) from the analysis, simulation, and real implementation and firstly proposes dynamic loading technique for a quadrature coupler and transmitting/receiving switch module to minimize a patient mismatching and enhance a system reliability. Also, we designed and implemented the quadrature coupler and transmitting/receiving switch module using microstrip. As a result, the SNR of our MRI system using the microstrip quadrature coupler and transmitting/receiving switch module with dynamic load increases 3 dB compared with the old one using USA quadrature switch. Also, the power capability of quadrature coupler and transmitting/receiving switch module is 5-kw peak power. Considering power loss and reduction of size, we used a RT/duroid 6010 substrate with high permittivity and for simulation we use Compact Software.

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Determination of Pantothenic acid in Fortified Foods by HPLC (시판 영양강화식품중 판토텐산의 분석)

  • 최윤주;장재희;박혜경;박건상;구용의;황인경;김대병
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.33 no.2
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    • pp.381-385
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    • 2004
  • This study was conducted to develop an HPLC method for determining pantothenic acid in fortified foods which has typically been determined by microbiological assay (MBA) according to AOAC and Korean Food Code approved methods. Pantothenic acid was determined by reversed-phase ion-pair HPLC using UV absorption (200 nm) after extraction with 20 mM potassium phosphate solution by sonication. The recovery of spiked samples and detection limit (LOD) by HPLC were 83.5∼109.6% and 0.5 ppm (mg/kg), respectively. The LOD of the microbiological assay (MBA) was much lower than that of HPLC. The concentrations of pantothenic acid analyzed in all tested samples (n=13) confirmed compliance with declared label claims. The range of recovery ratio by the HPLC method when compared to the microbiological assay was 91.9∼117.6%. There was not significant difference (p<0.01) between the HPLC and MBA methods and the equation of the regression curve was y=1.1428x-0.2269 (r=0.9842). This proposed HPLC method for determining pantothenic acid appears to be suitable for determining pantothenic acid concentrations above 0.25 mg/100 g in fortified foods.

Development of Immuno-Analytical System for Microbial Cells by using Dot-Blotter (Dot-Blotter 진공 포획방식에 의한 미생물세포 면역분석시스템의 개발)

  • 목락선;하연철;윤희주;백세환
    • KSBB Journal
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    • v.14 no.1
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    • pp.82-90
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    • 1999
  • In order to eventually fabricate an analytical system for infectious microorganisms, we synthesized major immunochemical components, utilized them for the construction of model system, and investigated an assay concept for bacterial whole cells. For the preparation of system components, a polyclonal antibody, against Salmonella thompson as model analyte, purified by immuno-affinity chromatography was used to chemically link to streptavidin or an enzyme, horseradish peroxidase(HRP). The antibody and streptavidin was modified with sulfosuccinimidyl 4-[N-maleimidomethyl]cyclohexane-1-carboxylate and N-succinimidyl-3-[2-pyridyldithio]propionate(subsequently activated by dithiotheritol), respectively. The modified components were reacted to synthesize antibody-streptavidin conjugates which were then purified on a two-layer chromatography column of diaminobiotin gel and Sephadex G-100. For antibody-HRP conjugates, HRP molecules were activated by $NalO_4$ oxidation and then coupled to immunoglobulin. After stabilizing with ($NaCNBH_3$, the conjugates were purified by size exclusion chromatography on Biogel A5M column. To devise a model system, such produced components were combined with a dot-blotter in which a nitrocellulose membrane($12{\mu}m$ pre size) with immobilized biotin was already located. The analyte (S. thompson cells) was reacted with the both antibody conjugates in a liquid phase, and the complexes formed were captured on the membrane surfaces by applying vacuum in the bottom compartment of the blotter to invoke biotin-streptavidin reaction. Under optimal conditions, the system enabled to identify the analytical concept for bacterial whole cells, and the lower limit of detection was approximately $1{\mu}g/m{\ell}$($10^5-10^6$ cells/m$m{\ell}$). The controlling factors were the concentrations of each antibody conjugate that caused agglutination in the presence of analyte as they increased.

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Effects of Sugars Addition in Alcohol Fermentation of Oriental Melon (첨가 당의 종류가 참외의 알코올발효에 미치는 영향)

  • Jo, Yong-Jun;Jang, Se-Young;Kim, Ok-Mi;Park, Chan-Woo;Jeong, Yong-Jin
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.39 no.9
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    • pp.1359-1365
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    • 2010
  • This study investigated effects of types of added sugar on alcohol fermentation of oriental melon. According to the results, pH was not significantly different according to types of added sugar and fermentation process. Total acidity increased with fermentation process in all groups by recording around 1.4% at the ninth day of fermentation. For sugar content, its initial level was $22^{\circ}Brix$, and alcohol fermented oriental melon fluids added by sucrose, fructose and glucose recorded similar levels or $6.6{\sim}6.8^{\circ}Brix$ while the fluids added by honey and fructo-oligosaccharide showed a slightly higher level or $8.1^{\circ}Brix$ at the ninth day of fermentation. Although free sugar content was different in the early phase of fermentation according to types of added sugar such as sucrose, fructose and glucose, it reduced with fermentation process to nearly non-detection at the ninth day of fermentation. As organic acids, lactic acid and acetic acid were observed in all phases of fermentation and their contents became higher gradually with fermentation process. Alcohol content showed the highest level in alcohol fermented oriental melon fluid added by sucrose by recording 12.80% and was relatively low in the fluids added by fructose and oligosaccharide. For alcohol, acetaldehyde, n-propanol and iso- amylalcohol contents were not significantly different according to types of added sugar and methanol content was the lowest in the fluid added by fructose by recording 84.99 ppm.