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Monitoring of Veterinary Antibiotics in Agricultural Soils using Liquid Chromatography Coupled with Tandem Mass Spectrometry (LC-MS/MS를 이용한 농경지 토양 중 항생제 모니터링)

  • Lee, Young-Jun;Choi, Jeong-Heui;Chung, Hyung Suk;Lee, Han Sol;Park, Byung-Jun;Kim, Jang-Eok;Shim, Jae-Han
    • Korean Journal of Environmental Agriculture
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    • v.35 no.3
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    • pp.166-174
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    • 2016
  • BACKGROUND: The current study developed a monitoring method of 6 veterinary antibiotics (amoxicillin, ampicillin, enrofloxacin, tetracycline, chlortetracycline, oxytetracycline) in agricultural soils using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive electrospray ionization mode.METHODS AND RESULTS: Sample preparation was carried out using acidic acetonitrile and citrate salts followed by purification with dispersive solid phase extraction (d-SPE). Separation on Eclipse Plus C18 column was conducted in gradient of the mobile phase, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations expressed as the coefficient of determination was good with R2≥0.9900. The limit of quantifications (LOQs) ranged from 0.5 to 10 μg/kg for all analytes. Analysis of 51 agricultural soil samples taken in the Republic of Korea revealed concentrations less than 1.9 μg/kg for enrofloxacin, 75.5 μg/kg for chlortetracycline.CONCLUSION: The method was successfully applied to monitor 6 veterinary antibiotics from 51 field incurred agricultural soil samples in 17 provincial areas throughout the Republic of Korea. The developed method was simple, easy, and versatile and can be used for monitoring various veterinary antibiotics in soil.

Development and Validation of an Analytical Method for Glucuronolactone in Energy Drinks by Hydrophilic Interaction Liquid Chromatography-electrospray Tandem Mass Spectrometry

  • Oh, Mi Hyune;Lim, Moo Song;Chai, Jeung Young;Kim, Eun Jung;Cho, Joong Hoon;Lim, Chul Joo;Choi, Sun Ok
    • Journal of Food Hygiene and Safety
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    • v.32 no.2
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    • pp.89-95
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    • 2017
  • A rapid, sensitive analytical method for glucuronolactone in beverages was developed and validated using hydrophilic interaction liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HILIC-ESI-MS/MS). To determine the optimum analytical conditions for glucuronolactone, three different kinds of HILIC columns and two mobile phases with different pH values were examined. An amide-bonded stationary phase with a pH 9 acetonitrile-rich mobile phase was the best condition in terms of column retention, ESI-MS/MS response area, and signal-to-noise ratio. After extraction, glucuronolactone was separated through the HILIC amide column and detected by negative ESI-MS/MS in selected reaction monitoring (SRM) mode. Nine energy drinks sold in Korea were spiked with glucuronolactone at a concentration of 5 ng/mL; the Monster $Energy^{TM}$ sample showed the smallest peak area and its signal-to-noise ratio was used for method validation. Good linearity was obtained in the concentration range from 20 to 1500 ng/mL with a correlation coefficient > 0.998. The developed method had a limit of detection (LOD) of 6 ng/mL and a limit of quantitation (LOQ) of 20 ng/mL. The recovery of this method at concentration of 20, 100, 500, and 1000 ng/mL was 96.3%-99.2% with relative standard deviations (RSD) of 1.6%-14.0%. A reproducibility precision assessment at concentration of 100 and 500 ng/mL was carried out among three laboratories. The recovery of that evaluation was 95.1%-102.3% with RSD of 2.7%-7.0%. An analysis of variance indicated that there was no difference between the recovery results of the three laboratories at the 5% significance level. The validated method is applicable to inspecting beverages adulterated with glucuronolactone in Korea.

Ocean Circulation Model ing of East Sea for Aquatic Dispersion of Liquid Radioactive Effluents from Nuclear Power Plants (원전 액체 방사성 유출물 해양확산 평가를 위한 동해 해수순환 모델링)

  • Chung Yang-Geun;Lee Gab-Bock;Bang Sun-Young;Lee Ung-Gwon;Lee Yong-Sun
    • Proceedings of the Korean Radioactive Waste Society Conference
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    • 2005.11a
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    • pp.321-331
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    • 2005
  • Recently. three-dimensional models have been used for aquatic dispersion of radioactive effluents in relation to nuclear power plant siting based on the Notice No. 2003-12 'Guideline for investigating and assessing hydrological and aquatic characteristics of nuclear facility site' of the Ministry of Science and Technology (MOST) in Korea. Several nuclear power plants have been under construction or planed. which are Shin-Korl Unit 1 and 2, Shin-Wolsong Unit 1 and 2, and Shln-Ulchin Unit 1 and 2. For assessing the aquatic dispersion of radionuclides released from the above nuclear power plants, it is necessary to know the coastal currents around sites which are affected by circulation of East Sea. In this study, a three dimensional hydrodynamic model for the circulation of the East Sea of Korea has been developed as the first Phase, which Is based on the RIAMOM. The model uses the primitive equation with hydrostatic approximation, and uses Arakawa-B grid system horizontally and Z-coordinate vertically. Model domain is $126.5^{\circ}E\;to\;142.5^{\circ}E$ of east longitude and $33^{\circ}N\;and\;52^{\circ}N$ of the north latitude. The space of the horizontal grid was $1/12^{\circ}$ to longitude and latitude direction and vortical level was divided to 20. This model uses Generalized Arakawa Scheme. Slant Advection, and Mode-Splitting Method. The input data were from JODC, KNFRDI, and ECMWF. The model ing results are in fairly good agreement with schematic patterns of the surface circulation in the East Sea The local current model and aquatic dispersion model of the coastal region will be developed as the second phase. The oceanic dispersion experiments will be also tarried out by using ARGO Drifter around a nuclear pelter plant site.

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Traveling-wave Ti:LiNbO3 optical modulator capable of complete switching (완전 스위칭이 가능한 Ti:LiNbO3 진행파 광변조기)

  • 곽재곤;김경암;김영문;정은주;피중호;박권동;김창민
    • Korean Journal of Optics and Photonics
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    • v.14 no.5
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    • pp.545-554
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    • 2003
  • Design of the optical modulator composed of a three-waveguide coupler and CPW traveling-wave electrodes was carried out. Switching phenomena of three-waveguide couplers were analyzed by using the coupled mode theory, and the coupling-lengths of the devices were calculated by means of the FDM. CPW traveling-wave electrodes were analysed by the CMM and SOR simulation technique in order to find the conditions of phase-velocity and impedance matching. Traveling-wave modulators were fabricated on z-cut LiNbO$_3$ substrate. Ti was in-diffused in LiNbO$_3$ to make waveguides and Au electrodes were built on the waveguides by the electrolyte technique. The fabricated modulator chip was end-polished, pig-tailed and packaged in a brass mount with K-connector. The insertion loss and the switching voltage of the optical modulator were about 4㏈ and 19V, respectively. Network analyzer was used to obtain the S parameter and the corresponding RF response. From the measurement, parameters of the traveling-wave electrodes were extracted to be Z$_{c}$= 45 Ω, N$_{eff}$=2.20, and $\alpha$$_{0}$=0.055/cm√GHZ. The measured optical response R($\omega$) was compared with the theoretically estimated one, showing both responses agree well. The measurement results revealed that 3㏈ bandwidth turned out to be about 13 GHz.

Development of Simultaneous Analytical Method of Veterinary Antibiotics in Manure using Liquid Chromatography Coupled with Tandem Mass Spectrometry (LC-MS/MS를 이용한 퇴비 및 액비 중 항생제 동시 분석법 개발)

  • Chung, Hyung Suk;Lee, Young Jun;Lee, Han Sol;Rahman, Md. Musfiqur;Kabir, Md. Humayun;Park, Byung-Jun;Kim, Jang-Eok;Shim, Jae-Han
    • Korean Journal of Environmental Agriculture
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    • v.36 no.3
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    • pp.201-210
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    • 2017
  • BACKGROUND: The current study was to monitor of 9 veterinary antibiotics (ceftiofur, clopidol, florfenicol, sulfamethazine, sulfamethoxazole, sulfathiazole, tetracycline, tiamulin, and tylosin) in manure using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive and negative electrospray ionization mode. METHODS AND RESULTS: Sample preparation was carried out using Mcllvaine buffer and citrate salts to adjust the pH of the sample followed by purification with dispersive solid phase extraction (d-SPE). Separation of analytes during LC-MS/MS analysis was conducted using an Eclipse Plus $C_{18}$ column and the mobile phase was in gradient mode with, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations of all tested antibiotics was good, with $R^2$ determination coefficients ${\geq}0.9920$. The limit of detection (LOD) and quantifications (LOQ) were $0.1-67.0{\mu}g/kg$ and $0.4-200.0{\mu}g/kg$, respectively. Analysis of 13 solid and liquid manure samples taken from the Republic of Korea revealed concentrations less than $0.7{\mu}g/kg$ for tiamulin, $1497.6{\mu}g/kg$ for sulfamethazine. CONCLUSION: To monitor 9 veterinary antibiotics from manure samples in 13 provincial areas throughout the Republic of Korea, an analytical method was developed. The developed method was fully validated and successfully applied for monitoring various veterinary antibiotics in manure samples.

Intercomparison of Satellite Data with Model Reanalyses on Lower- Stratospheric Temperature (하부 성층권 온도에 대한 위성자료와 모델 재분석들과의 비교)

  • Yoo, Jung-Moon;Kim, Jin-Nam
    • Journal of the Korean earth science society
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    • v.21 no.2
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    • pp.137-158
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    • 2000
  • The correlation and Empirical Orthogonal Function (EOF) analyses over the globe have been applied to intercompare lower-stratospheric (${\sim}$70hPa) temperature obtained from satellite data and two model reanalyses. The data is the19 years (1980-98) Microwave Sounding Unit (MSU) channel 4 (Ch4) brightness temperature, and the reanalyses are GCM (NCEP, 1980-97; GEOS, 1981-94) outputs. In MSU monthly climatological anomaly, the temperature substantially decreases by ${\sim}$21k in winter over southern polar regions, and its annual cycle over tropics is weak. In October the temperature and total ozone over the area south of Australia remarkably increase together. High correlations (r${\ge}$0.95) between MSU and reanalyses occur in most global areas, but they are lower (r${\sim}$O.75) over the 20-3ON latitudes, northern America and southern Andes mountains. The first mode of MSU and reanalyses for monthly-mean Ch4 temperature shows annual cycle, and the lower-stratospheric warming due to volcanic eruptions. The analyses near the Korean peninsula show that lower-stratospheric temperature, out of phase with that for troposphere, increases in winter and decreases in summer. In the first mode for anomaly over the tropical Pacific, MSU and reanalyses indicate lower-stratospheric warming due to volcanic eruptions. In the second mode MSU and GEOS present Quasi-Biennial Oscillation (QBO) while NCEP, El Ni${\tilde{n}}$o. Volcanic eruption and QBO have more impact on lower-stratospheric thermal state than El Ni${\tilde{n}}$o. The EOF over the tropical Atlantic is similar to that over the Pacific, except a negligible effect of El Ni${\tilde{n}}$o. This study suggests that intercomparison of satellite data with model reanalyses may estimate relative accuracy of both data.

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Sports Injuries in College Taekwondo Players: Retrospective Analysis of 47 Players (대학 태권도 선수들에서의 스포츠 손상: 47명에 대한 후향적 연구)

  • Jung, Hong-Geun;Park, Hee-Gon;Kim, Jong-Phil;Kim, You-Jin;Kim, Ki-Choul;Kim, Young-In;Lee, Sang-Min
    • Journal of Korean Orthopaedic Sports Medicine
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    • v.5 no.1
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    • pp.69-74
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    • 2006
  • Purpose: To perform the retrospective analysis of the sports injuries sustained by the college Taekwondo athletes in the respect of the injury patterns, mechanism of injury and clinical outcome Materials and Methods: This study is based on 47 out of 49 college Takwondo athletes, who had experienced the Takwondo related musculoskeletal injuries severe enough to visit the clinic for medical treatment. The mean age at the time of injury was 18.8 years and 39 were males and 8 females. The Taekwondo career was average 9.6 years and the injuries were sustained at average 6.7 years of their career. The injuries were analyzed by the detailed interview with thorough physical examination. Results: Forty-seven Taekwondo athletes in the study experienced average 1.8 injury/person (total 85 cases) with 26 persons of one time experience(55.3%), 11 persons of 2 times(23.4%),4 persons of 3 times (8.5%),5 persons of 4 times (10.6%) and 1 person of 5 times (2.2%). Injuries occurred during training in 50 cases (58.8%), while during match in 35 cases (41.2%). Injuries occurred during the attack phase of the match are 26 cases (31.7%) while 49 cases (57.6%) during the defense phase. As for the pattern of injury, fracture was the most common with 49 cases (57.6%), followed by ligament injury with 21 cases (24.7%). The upper extremity injuries were 32 cases (37.7%) while the lower extremity injuries were 44 cases (51.8%) Mode of medical treatment were operation in 15cases(17.7%), cast in 21 cases(24.7%), splint in 33 cases (38.8%), physical therapy in 15cases(17.7%) and acupuncture in 1 case(1.1%) Conclusion: Almost all the college Taekwondo athletes (96%) experienced sports injuries severe enough to receive medical treatments with the fracture being the most common injury pattern. The injuries occurred more commonly during the defense phase of the competition.

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Development and Validation of the Determination of Sorafenib in Human Plasma using Tandem Mass Spectrometry Coupled with Liquid Chromatography (고속액체크로마토그래피 텐덤질량분석기법을 이용한 사람 혈장 내 소라페닙 농도분석법의 개발 및 검정)

  • Park, Daejin;Lee, Sunggon;Kim, Woomi
    • Journal of Life Science
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    • v.22 no.11
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    • pp.1456-1462
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    • 2012
  • Sorafenib is a multikinase inhibitor and an oral anticancer drug approved for the treatment of patients with advanced renal cell carcinoma and those with unresectable hepatocellular carcinoma. The purpose of this study was to develop an efficient method of the determination of sorafenib in human plasma using tandem mass spectrometry coupled with liquid chromatography (LC/MS/MS) and validate the method by the guidelines of the Korean Food and Drug Administration (KFDA). Plasma samples ($100{\mu}l$) were added with chlorantraniliprole as an internal standard and then mixed with the 0.1% formic acid-containing extraction solution composed of isopropyl alcohol and ethyl acetate (1:4, v/v). After centrifugation, the supernatant was concentrated at $45^{\circ}C$ under negative pressure and centrifugal force. The residue was reconstituted with a mobile phase and injected into the HPLC instrument using a reverse phase Waters XTerra$^{TM}$ C18 column (particle size $3.5{\mu}m$). Liquid chromatography was carried out within the run time of 5 min using a mobile phase composed of buffer (0.1% formic acid and 10 mM ammonium formate), methanol, and acetonitrile (1:6:3, v/v/v). The analytes were monitored by tandem mass spectrometry in the multiple reaction monitoring method programmed to detect sorafenib at 'm/z 465.2 ${\rightarrow}$ 252.5' and chlorantraniliprole at 'm/z 484.4 ${\rightarrow}$ 286.2' with positive electrospray ionization mode ($ES^+$). The result showed the proper linearity ($r^2$ > 0.99) over the range of 2,000-5,000 ng/ml with good accuracy (90.7-103.9%) and precision (less than 10%). The newly developed method using LC/MS/MS was validated by the guideline of KFDA and identified as more sensitive compared to the previous methods.

Development of Differential Diagnosis and Treatment Method of Reproductive Disorders Using Ultrasonography in Cows II. Differential Diagnosis of Subestrous Dairy Cows (초음파검사에 의한 소의 번식장애 감별진단 및 치료법 개발 II. 무발정우의 감별진단)

  • 강병규;최한선;강현구;오기석;서동호;손창호;서국현
    • Journal of Veterinary Clinics
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    • v.15 no.2
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    • pp.307-318
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    • 1998
  • Accuracy of rectal palpation and ultrasonography for differential diagnosis of subestrous dairy trows were investigatedl using the result of pIRsma progesterone assay. The ovaries were examined 2 times of 10 days interval in 520 posearom and postinsemination subestroHs dairy cows, using rectal palpation and B-mode transrectal ultrasonography. The results of rectal palpation, ultrasonographic examination and measurement of plasma progesterone profiles in 520 subestrous dairy cows were silent brat or error of estrus detection 303 (58.3%), persistent corpus luteum 59 (11.3%), follicular cyst 37 (7.1%), luteal cyst 16 (3.1%), inactive ovary 9 (1.7%), granulosa tumor 1 (0.2%), hydmsalphinx 1 (0.2%), endomehris 81 (15.6%), pyometra 12 (2.3%) and mummified fetus 1 (0.2%), respectively. Accuncy of rectal palpation and ultrasonography for diagiosing ovarian disordeir based on plasma progesterone profiles were silent heat or error of estrus detection 80.5% and 96.7%$\boxUl$ persistent corpus luteum 57.6% and 94.9%, follicular cyst 62.5% and 91.9%1 luteal cyst 62.5% and 87.5%, maclive ovary 55.6% and 88.9% and granulosa cell tumor 100% and 100%, respectively. Acnuucy of rectal palpation for diagnosing uterine disorders based on ultrasonography was pyometra 75.0%1 endometritis 51.9% and mummified fetus 100%, respectively. Cbaracteristic ultrasonographic appearances of ovaries in subestrous dairy cows were as follows; Silent heat or error of estrus detection: anechoic follicle or hypoechoic corpus luteum than ovarian stroma was alternately present on Day 0 (first examination) and Day 10. Follicular cyst: uniformly nonechogenic ovarian structure $\geq $ 25 mm in diameter with a wall < 3 mm was present in ipsilateral on Day 0 and Day 10. Luteal cyst: luteal cyst was similar to follicular cysts but thickness of cystic wall was $\geq $ 3 mm. Inactive ovary : structures within ovaries was not present on Day 0 Bnd Day 10. Characteristic uthssonograpsc appearances of uterus in subestrous dairy cows were as follows; Endometritis: characterized by uterine lumen containing fluid in which 'snowy'echogenic particles art suspended. Pyometra: ultrasonographic appearance of pyometra was diffuse echogenic particles distributed in fluid within the distended uterus, and a thickened uterine wall. These results indicated that ultrasonography was practical far diagnosing reproductive disorders. To diagnosing ovarian disorders, ultrasonography should be carried out 2 times of 10 days interval and rndometritis should be differentiated with uterus of luteal phase in normal cycling cows.

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3-Dimensional Numerical Analysis of Air Flow inside OWC Type WEC Equipped with Channel of Seawater Exchange and Wave Characteristics around Its Structure (in Case of Regular Waves) (해수소통구를 구비한 진동수주형 파력발전구조물 내에서 공기흐름과 구조물 주변에서 파랑특성에 관한 3차원수치해석(규칙파의 경우))

  • Lee, Kwang Ho;Lee, Jun Hyeong;Jeong, Ik Han;Kim, Do Sam
    • Journal of Korean Society of Coastal and Ocean Engineers
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    • v.30 no.6
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    • pp.242-252
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    • 2018
  • It is well known that an Oscillating Water Column Wave Energy Converter (OWC-WEC) is one of the most efficient wave absorber equipment. This device transforms the vertical motion of water column in the air chamber into the air flow velocity and produces electricity from the driving force of turbine as represented by the Wells turbine. Therefore, in order to obtain high electric energy, it is necessary to amplify the water surface vibration by inducing resonance of the piston mode in the water surface fluctuation in the air chamber. In this study, a new type of OWC-WEC with a seawater channel is used, and the wave deformation by the structure, water surface fluctuation in the air chamber, air outflow velocity from the nozzle and seawater flow velocity in the seawater channel are evaluated by numerical analysis in detail. The numerical analysis model uses open CFD code OLAFLOW model based on multi-phase analysis technique of Navier-Stokes solver. To validate model, numerical results and existing experimental results are compared and discussed. It is revealed within the scope of this study that the air flow velocity at nozzle increases as the Ursell number becomes larger, and the air velocity that flows out from the inside of the air chamber is larger than the velocity of incoming air into the air chamber.