• Title/Summary/Keyword: phase detection

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Determinations of Toltrazuril and Toltrazuril Sulfone Levels in Olive Flounder Paralichthys olivaceus Samples Using Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry (LC-MS/MS를 이용한 넙치(Paralichthys olivaceus)시료의 톨트라주릴 및 톨트라주릴 설폰 분석)

  • Hong, Do Hee;Kim, Ah Hyun;Lee, Ka Jeong;Yoon, Minchul;Son, Kwang Tae;Kim, Myoung Sug;Kim, Na Young;Jung, Sung Hee;Jo, Mi Ra
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.52 no.5
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    • pp.461-467
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    • 2019
  • Several studies investigating the prevention and treatment of external parasites in farmed olive flounder Paralichthys olivaceus have found that the anticoccidial agent toltrazuril sulfone is an effective antiparasitic. Prior to undertaking a full-scale study, we developed analytical methods to detect the levels of toltrazuril and toltrazuril sulfone in farmed flounder samples using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-MS/MS). This analysis showed that LC-MS/MS changed the mobile phase and collision energy of toltrazuril and toltrazuril sulfone. This was validated using established conditions. Sample pre-treatment for this process involved extraction with dichloromethane and purification by liquid-liquid extraction in formic acid, acetonitrile, and h-hexane, followed by determination of all compounds by LC-MS/MS. Separation was achieved within 10 min by gradient elution using a Capcell Pak C18 ($3.0{\mu}m$, $100{\times}2.0mm$) analytical column (Shiseido UG 120V) with a mixture of 0.1% (v/v) formic acid and acetonitrile. Multiple reaction monitoring was used for selective detection of toltrazuril and toltrazuril sulfone. This method yields satisfactory results for linearity, precision, and limits of quantification. Therefore, the method established in our study will serve as a basis for further research on parasite control by toltrazuril and toltrazuril sulfone.

Development of Individual Residue Analysis Method for Cyanazine in Agricultural Commodities as an Unregistered Herbicide in Korea (국내 미등록 제초제 cyanazine의 농산물 중 개별 잔류분석법 개발)

  • Choung, Myoung-Gun;Im, Moo-Hyeog
    • Journal of the Korean Society of International Agriculture
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    • v.30 no.4
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    • pp.339-346
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    • 2018
  • Cyanazine is a member of the triazine family of herbicides. Cyanazine is used as a pre- and post-emergence herbicide for the control of annual grasses and broadleaf weeds. This experiment was conducted to establish a determination method for cyanazine, as domestic unregistered pesticide, residue in major agricultural commodities using HPLC-DAD/MS. Cyanazine was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and partitioned to dichloromethane for remove polar extractive in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized florisil column chromatography. On a $C_{18}$ column in HPLC, cyanazine was successfully separated from co-extractives of sample, and sensitively quantitated by diode array detection at 220 nm. Accuracy and precision of the proposed method was validated by the recovery experiment on every major agricultural commodity samples fortified with cyanazine at 3 concentration levels per agricultural commodity in each triplication. Mean recoveries were ranged from 83.6 to 93.3% in five major representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation(LOQ) of cyanazine was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring(SIM) technique was also provided to clearly identify the suspected residue.

Immobilization of As and Pb in Contaminated Soil Using Bead Type Amendment Prepared by Iron NanoparticlesImpregnated Biochar (철 나노 입자가 담지된 바이오차 기반 비드 형태 안정화제를 이용한 비소 및 납 오염토양의 안정화)

  • Choi, Yu-Lim;Kim, Dong-Su;Kang, Tae-Jun;Yang, Jae-Kyu;Chang, Yoon-Young
    • Journal of Environmental Impact Assessment
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    • v.30 no.4
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    • pp.247-257
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    • 2021
  • In this work, Iron Nano-Particles Impregnated BioChar/bead (INPBC/bead) soil amendment was developed to increase biochar's reactivity to As in soil and preventing possible wind loss. Prior to preparation of INPBC/bead, INPBC was produced utilizing lignocellulosic biomass and Fe(III) solution in a hydrothermal method, followed by a calcination process. Then, the bead type amendment, INPBC/bead was produced by cross-linking reaction of alginate with INPBC. FT-IR, XRD, BET, and SEM-EDS analyses were utilized to characterize the as-synthesised materials. The particle size range of INPBC/bead was 1-4 mm, and different oxygen-containing functional groups and Fe3O4 crystalline phase were produced on the surface of INPBC/bead, according to the characterization results. The soil cultivation test was carried out in order to assess the stabilization performance of INPBC/bead utilizing As and Pb-contaminated soil obtained from an abandoned mining location in South Korea. After 4 weeks of culture, TCLP and SPLP extraction tests were performed to assess the stabilization efficacy of the amendment. The TCLP and SPLP findings revealed that raising the application ratio improved stabilizing efficiency. The As stabilization efficiency was determined to be 81.56 % based on SPLP test findings for a 5% in (w/w) INPBC/bead treatment, and the content of Pb in extracts was reduced to the limit of detection. According to the findings of this study, INPBC/bead that can maintain pH of origin soil and minimize wind loss might be a potential amendment for soil polluted with As and heavy metals.

Optimization for I-129 analytical method of radioactive waste sample using a high-temperature combustion tube furnace (고온연소로를 이용한 방사성 폐기물 내 I-129 정량 분석법 최적화 연구)

  • Chae-yeon, Lee;Jong-Myoung, Lim;Hyuncheol, Kim;Ji-Young, Park;Jin-Hong, Lee
    • Analytical Science and Technology
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    • v.35 no.6
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    • pp.256-266
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    • 2022
  • It is important to determine the concentration of long-lived radionuclides (e.g., 129I) in nuclear waste to ensure safety when handling it. To analyze nuclides in a solid sample (e.g., concrete and soil), it is essential to effectively separate and purify the nuclides of interest in the sample. This study reports the comprehensive efforts made to validate the analytical procedure for 129I detection in solid samples, using a high-temperature combustion furnace. 129I volatilized from the sample collected in 0.01 M HNO3 solution with a reducing agent (e.g., NaHSO3) and was rapidly measured by ICP-MS. Analytical conditions, such as pyrolysis temperature and types of mobile phase gas, catalyst, and trapping solution, were optimized to obtain a high recovery rate of spiked 129I. Finally, the optimized method was applied for the simultaneous analysis of other volatile radionuclides, such as 3H and 14C. The performance test results for the optimized method confirmed that the LSC (for 3H and 14C) and ICP-MS (for 129I) measurements, with the separation of volatile nuclides using a high-temperature combustion furnace, were reliable.

Analysis Method of Surfactants for Identification of Residue Dishwashing Detergent (세척제 잔류량 확인을 위한 계면활성제 분석법 확립)

  • Park, Na-Youn;Lee, Sojeong;Kim, Jung Hoan;Kho, Younglim
    • Journal of the Korean Chemical Society
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    • v.65 no.6
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    • pp.433-440
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    • 2021
  • Surfactants are organic compounds that have both hydrophilic and non-polar parts in one molecule, classified as non-ion, anion, cation, and amphoteric surfactants according to the charge of hydrophilic parts in aqueous state. A trace amounts may remain when vegetables and fruits are washed using type1 detergent (Vegetable and fruit detergent), and there is a possibility of exposure to the human body through ingestion. This study developed the simultaneous analysis method for 5 surfactants with LC-MS/MS for analysis of detergent residues after washing vegetables and fruits with detergent. The mobile phase used distilled water and acetonitrile containing 50 mM ammonium formate and 0.1% formic acid and was analyzed using a gradient method using XBridge BEH C8 column. The accuracy of the established method was 83.9-112.1%, and the precision was less than 20%. The detection limit was 7.0 (SLS) to 29.0 (SLES-N3) ㎍/L, and the correlation coefficient (r2) of calibration line regression was greater than 0.99, it is considered suitable for the analysis of trace amounts of surfactant components remaining in vegetables and fruits.

A Study on the Improvement of Fire Evacuation Scenario Using Delphi Technique -Focus on The Mobile Application and psychology- (델파이 기법을 활용한 화재피난 시나리오 개선 연구- 모바일 어플리케이션과 재실자 심리를 중심으로 -)

  • Lee, Sang ki;Kim, Sung Hyun
    • Journal of Service Research and Studies
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    • v.12 no.2
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    • pp.23-37
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    • 2022
  • Based on the service scenario proposed by the existing Kim Tae-wan (2018) who can safely evacuate inmates with the help of a mobile application linked to a fire detection system in the event of a fire, the final purpose of this study is to develop the scenario by incorporating more realistic scenarios with mobile stimuli that can help them escape or act through the Delph In addition, to make the scenarios produced more realistic considering the structure and copper lines of a typical building, expert scenario verification and Delphi technique were applied to exclude unnecessary or impractical aspects of the existing scenarios. The results of the second Delphi survey showed that the primary psychology that could be seen at the time of the fire alarm were doubts, safety concerns and alarm, and the results of the second Delphi survey were analyzed, and the satisfaction of the content adequacy (CVR), convergence, and consensus was derived. Finally, this was applied to create a scenario in which a mobile application was assisted to evacuate the fire response phase. This study will allow the use of methods to increase the evacuation rate of those who are in the event of a fire.

Improvement of Reproductive Efficiency of Artificial Insemination Following Estrus Induction in Dog II. Semen Freezing and Artificial Insemination in Dog

  • Lee, Y. R.;S. Y. Choe
    • Proceedings of the Korean Society of Embryo Transfer Conference
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    • 2002.11a
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    • pp.92-92
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    • 2002
  • Considerable attention has been focused on the cryopreservation of semen and estrus induction in dog, as consequence of poor productivity caused by long anestrus period, in order to enhance the productivity of youngs and to preserve the breeds. The objectives of this study were to evaluate semen quality after cryopreservation and to evaluate the Pregnancy rate after insemination (AI). Fifty infertilie dogs (age 2∼3 years) were selected for the study and divided into three different estrus induction treatment groups. Group 1: dogs (n=15) were given clomifene (0.1 mg/kg) orally for five days at 12 hr intervals. Group 2: dogs (n=15) were given bromocriptine (50 $\mu\textrm{g}$/kg) orally for five days at 12 hr intervals, followed by single injection intravenously of 500 IU GnRH (Group 3, n=20) when pro-estrus occurred. The rates of pregnancy in estrus inducted dogs mated naturally compared to those inseminated artificially with ejaculated fresh semen and frozen-thawed semen. Estrus detection was performed using the method of vaginal smear and confirmed by the plasma progesterone assay. The ejaculated semen to freeze was exposed to a mixture of Tris extender with cryoprotectant (Trisma, 81 mM: TES, 209 mM: citric acid, 6 mM; glucose, 5 mM; glycerol, 8%) and cryopreserved gradually by slow-cooling at 17 cm above the surface of liquid nitrogen (LN$_2$) for 23 min. The motility of frozen-thawed spermatozoa was assessed by phase-contrast microscopy. To assess their viability and acrosome content, spermatozoa were stained with a vital stain and Fluorescence conjugated lectin Pisum Savitum Agglutinin (FITC/PAS), respectively. Pregnancy was confirmed by ultrasonograpy on day 25, 35 and 55 post insemination. The use of fresh semen, the pregnancy rates were observed 66.6, 66.6, 75.0 and 83.3% in natural estrus, clomifene induced, bromocriptine induced and a combination of GnRH and bromocriptine, respectively. The use of frozen-thawed semen, the pregnancy rates were observed 66.6, 33.3, 50.0 and 60.0% in natural estrus, clomifene induced, bromocriptine induced and a combination of GnRH and bromocriptine, respectively. No difference was observed in the number of offspring produced among natural estrus and treated groups inseminated with fresh or frozen-thawed semen. In conclusion, the pregnancy rate of dogs treated with a combination of GnRH and bromocriptine was more effective than use of clomifene or bromocriptine only. In addition, frozen-thawed semen can be used successfully far artificial insemination in dog.

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A comparative study of cavitation inception of naval ship's propeller using on-board noise and vibration signals (선체 부착 소음/진동 센서를 이용한 함정 추진기 캐비테이션 초생 분석 비교 연구)

  • Hongseok Jeong;Hanshin Seol
    • The Journal of the Acoustical Society of Korea
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    • v.42 no.3
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    • pp.243-249
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    • 2023
  • The occurrence of cavitation on the propeller is directly linked to the naval ship's survivability, and it is necessary to design a propeller shape that delays the cavitation inception. However, the propeller cavitation can occur under various operating conditions, thus it is important to identify whether the propeller cavitation exists during operation as well as in the design phase. To this end, it is necessary to use noise or vibration signals on board to monitor the cavitation inception. In this study, a hydrophone and an accelerometer were installed on the ship hull right above the propeller to compare the performance of analyzing cavitation inception between acoustic and vibration signals. Also, a high speed camera was used to visually observe the occurrence of cavitation through an observation window. The measured results showed that the spectral shapes between acoustic and vibration signals were different, but the level increases at each frequency band and the overall level of the frequency band from 1 kHz to 10 kHz showed a similar tendency. The Detection of Envelope Modulation On Noise (DEMON) analysis also showed similar results for both acoustic and vibration signals, confirming that both hydrophones and accelerometers can be utilized in the analysis of cavitation inception.

Levels of sulfonamides for animals in food (식품 중 설폰아마이드계 동물용의약품의 잔류실태)

  • Jeong, Jiyoon;Hong, Mooki;Choi, Dongmi
    • Analytical Science and Technology
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    • v.20 no.1
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    • pp.84-90
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    • 2007
  • To determine levels of 11 sulfonamides for animals in food, simultaneously, a selective method of high performance liquid chromatography with UV detector has been applied. The targets were sulfachlorpyridazine (SCP), sulfadiazine (SDZ), sulfadimethoxine (SDM), sulfisoxazole (SSX), sulfamerazine (SMZ), sulfamethazine (SMT), sulfamethoxazole (SMX), sulfamethoxypyridazine (SMP), sulfamonomethoxine (SMM), sulfaquinoxaline (SQX) and sulfathiazole (STZ). Food samples were beef, pork, chicken, milk and whole egg that were collected at the main 6 cities in Korea as Seoul, Busan, Daejon, Incheon, Mokpo and Gangneung. After homogenizing food samples with sodium phosphate solution and acetonitrile, it was extracted with n-hexane. The mobile phase gradient was a mixture of 5 mM potassium phosphate (pH 3.25) and methanol with a gradient ratio from 100:0 to 30:70. The UV wavelength was 270 nm. The overall recoveries were ranged from 75% to 95% and the limit of detection was minimum 0.004 mg/kg for SMT, and 0.007 mg/kg for STZ at signal/noise > 3, respectively. As results, sulfonamide drugs were not detected in most of the selected food samples, however, sulfamonomethoxine was detected in meat. The determined level of sulfamonomethoxine were 0.03 and 0.06 mg/kg for beef that were below the MRLs.

Determination of mandipropamid residues in agricultural commodities using high-performance liquid chromatography with mass spectrometry (고성능액체크로마토그래피를 이용한 농산물 중 Mandipropamid의 잔류분석법 확립)

  • Kwon, Chan Hyeok;Chang, Moon Ik;Im, Moo Hyeog;Choi, Hoon;Jung, Da I;Lee, Su Chan;Yu, Jin Young;Lee, Young Deuk;Lee, Jong Ok;Hong, Moo Ki
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.518-525
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    • 2008
  • Mandipropamid is a new mandelamide-type fungicide to control foliar Oomycete pathogens in some vegetables. An analytical method was developed to determine mandipropamid residues in agricultural commodities using high-performance liquid chromatography (HPLC) and liquid chromatography/mass spectrometry (LC/MS). Mandipropamid was extracted with methanol from grape, tomato, green pepper, Chinese cabbage and potato samples. The extract was diluted with saturated sodium chloride solution and distilled water, and dichloromethane partition was followed to recover the mandipropamid from the aqueous phase. Florisil column chromatography was employed to further remove interfering co-extractives prior to HPLC analysis. Reverse-phased HPLC was successfully applied to determine mandipropamid in sample extracts with the detection at its ${\lambda}_{max}$ (223 nm). Overall recoveries of mandipropamid from fortified samples averaged $99.8{\pm}1.7$ (n=6), $89.3{\pm}5.3$ (n=6), $98.7{\pm}2.2$ (n=6), $99.7{\pm}6.8$ (n=6) and $91.1{\pm}3.1$ (n=6) for grape, tomato, green pepper, Chinese cabbage and potato, respectively. Limit of quantification of the method was 0.02~0.04 mg/kg for all samples. A LC/mass spectrometry with selected-ion monitoring was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to determine the terminal residue of mandipropamid in agricultural commodities.