• Title/Summary/Keyword: Reaction monitoring

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Determination of Nitrovin in Fishery Products by Liquid Chromatography-tandem Mass Spectrometry (LC-MS/MS를 이용한 수산물 중 니트로빈의 정량분석법 개발 및 검증)

  • Kim, Joohye;Shin, Dasom;Kang, Hui-Seung;Jeong, Jiyoon;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.33 no.2
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    • pp.118-123
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    • 2018
  • The objective of this study was to develop a sensitive method for the identification and determination of nitrovin in fishery products by using a solid-phase extraction (SPE), as performed with a liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with a mixture of acetonitrile and water, and were then defatted with acetonitrile saturated hexane, after which further clean-up was accomplished with SPE on the hydrophilic-lipophilic balance (HLB) cartridges. The analytes were subsequently ionized in the positive mode of an electrospray ionization (ESI), and where thereby detected in a process of multiple reaction monitoring (MRM). The linearity (expressed as correlation coefficients) of the matrix calibration curves was > 0.985. The limit of the quantification for the nitrovin was measured at 0.001 mg/kg. The accuracy (expressed as average recovery) was noted between 72.1 and 122%. The precision (expressed as coefficient variation) was noted from 2.9 to 16.9%. According to the CODEX CAC/GL-71 guideline accuracy, precision, linearity, and limit of detection were determined in three matrices (which were flatfish, eel and shrimp). The proposed method was suitable for analyzing the associated nitrovin residues. This application and result can also be a factor to contribute to the non-detection drugs management in fishery products.

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.

Experiment and Assessment of Ascending Capability for Management of Exotic Fish Species (외래어종 관리를 위한 소상 실험 및 평가)

  • Kang, Joon-Gu;Kim, Jong-Tae
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.17 no.9
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    • pp.265-278
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    • 2016
  • In this study, an ascending capability experiment was performed with largemouth bass and bluegill, which are exotic fish species inhabiting (the freshwaters) in Korea. The experiment was performed by dividing the subject fish into four groups according to their size and at four flow rates for each group. The number of fish passing through a reference line was analyzed by recording videos, and their swimming and ascending capabilities were observed by the naked eye. The number of fish passing through the reference line did not include those returning downstream within five minutes due to the high flow rate. The flow rate used for the analysis was the mean of the flow rate values measured at the left bank, the right bank, and in the middle of the stream. The results showed that the number of exotic fish migrating upstream decreased as the flow rate increased, regardless of the species and size of the fish. The comparison between the fish species showed that the ascending capability of bass was higher than that of bluegill, but the difference was not significant when considering the difference in the size of the fish. In addition, the upper limit flow velocity allowing the ascending of the exotic fish species was 1.11 m/s, when considering the fish returning to the downstream after the upstream migration and experimental error. The results of the experiment may be used as fundamental data for the blocking of fish and the management of exotic fish species by means of a high flow rate current. Further experiments, verification, and monitoring may need to be conducted continuously to determine whether the fish are able to pass through the reference line at a high flow rate, when they attain a high or cruising velocity. Additionally, the reaction of the fish species should be investigated by considering the response to external forces as well as pressure differences due to the flow rate.

Arthralgia and Myalgia Associated with the Use of Bisphosphonate: An Active Monitoring Study (비스포스포네이트 제제 관련 관절통 및 근육통에 대한 지역 약국 약사 및 환자 능동적 모니터링)

  • Song, Jung-woo;Park, So-Hee;Yoon, Dongwon;Lee, Mo-Se;Lee, Jung-Min;Kim, Na-Young;Kim, Young-Wook;Lee, Ju-Yeun;Shin, Ju-Young
    • Korean Journal of Clinical Pharmacy
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    • v.31 no.3
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    • pp.180-187
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    • 2021
  • Objective: We investigated arthralgia and myalgia associated with the use of oral bisphosphonate (BP) by conducting a survey of patient. Methods: The pharmacists conducted a survey between 1 Oct 2019 and 30 Sep 2020 among patients who were dispensed BP in community pharmacies to assess their demographic and medical characteristics, and their experiences with, and process for pain. Logistic regression analyses were performed to find the risk factors associated with the pain, and the odds ratios (OR) and 95% confidence intervals (CI) were determined. Results: A total of 160 patients who used BP participated in the survey (74 [46.3%] used risedronate; 61 [38.1%] used alendronate; 23 [14.4%] used ibandronate), and 20 (12.5%) of them experienced pain. Significant statistical differences of the characteristics between patients who experienced pain or not were observed regarding menopause, and parity. Compared with women who had one or two parity, women who had more than three parity were associated with the decreased risk of pain (OR, 0.24; 95% CI, 0.04-0.98). Moreover, steady exercise was associated with the decreased risk of pain compared to less exercise (OR, 0.37; 95% CI, 0.14-0.98). Conclusion: Our findings suggest that the risk of pain in BP-treated patients might be different regarding the different ingredients of BP, and dosing frequency. This survey highlights a need for a further safety research to understand the factors influencing the pain associated with the BP treatment.

Changes of carbon-13 Isotope of Dissolved Inorganic Carbon Within Low-pH CO2-rich Water during CO2 Degassing (pH가 낮은 탄산수의 CO2 탈기에 따른 용존탄소동위원소 변화)

  • Chae, Gitak;Yu, Soonyoung;Kim, Chan Yeong;Park, Jinyoung;Bang, Haeun;Lee, Inhye;Koh, Dong-Chan;Shinn, Young Jae;Oh, Jinman
    • Journal of Soil and Groundwater Environment
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    • v.24 no.3
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    • pp.24-35
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    • 2019
  • It is known that ${\delta}^{13}C_{DIC}$ (carbon-13 isotope of dissolved inorganic carbonate (DIC) ions) of water increases when dissolved $CO_2$ degases. However, ${\delta}^{13}C_{DIC}$ could decrease when the pH of water is lower than 5.5 at the early stage of degassing. Laboratory experiments were performed to observe the changes of ${\delta}^{13}C_{DIC}$ as $CO_2$ degassed from three different artificial $CO_2$-rich waters (ACWs) in which the initial pH was 4.9, 5.4, and 6.4, respectively. The pH, alkalinity and ${\delta}^{13}C_{DIC}$ were measured until 240 hours after degassing began and those data were compared with kinetic isotope fractionation calculations. Furthermore, same experiment was conducted with the natural $CO_2$-rich water (pH 4.9) from Daepyeong, Sejong City. As a result of experiments, we could observe the decrease of DIC and increase of pH as the degassing progressed. ACW with an initial pH of 6.4, ${\delta}^{13}C_{DIC}$ kept increasing but, in cases where the initial pH was lower than 5.5, ${\delta}^{13}C_{DIC}$ decreased until 6 hours. After 6 hours ${\delta}^{13}C_{DIC}$ increased within all cases because the $CO_2$ degassing caused pH increase and subsequently the ratio of $HCO_3{^-}$ in solution. In the early stage of $CO_2$ degassing, the laboratory measurements were well matched with the calculations, but after about 48 hours, the experiment results were deviated from the calculations, probably due to the equilibrium interaction with the atmosphere and precipitation of carbonates. The result of this study may be not applicable to all natural environments because the pressure and $CO_2$ concentration in headspace of reaction vessels was not maintained constant as well as the temperature. Nevertheless, this study provides fundamental knowledge on the ${\delta}^{13}C_{DIC}$ evolution during $CO_2$ degassing, and therefore it can be utilized in the studies about carbonated water with low pH and the monitoring of geologic carbon sequestration.

Monitoring of viruses in wild walleye pollock (Gadus chalcogrammus) population in Korea (국내 자연산 명태(Gadus chalcogrammus) 집단의 바이러스 모니터링)

  • Seo, Hyun-Joon;Nam, U-Hwa;Kim, Jeong-Ho
    • Journal of fish pathology
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    • v.31 no.2
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    • pp.71-79
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    • 2018
  • Wild walleye pollock were caught from Goseong, The East Sea of Korea and examined for the existence of several fish pathogenic viruses; viral hemorrhagic septicemia virus (VHSV), nervous necrosis virus (NNV) and marine birnavirus (MABV). We collected 1,253 wild walleye pollock in total during February 2015 and August 2018. 324 spleen sample sets and 259 brain sample sets were made, and examined for the existence of the viruses mentioned above by reverse transcriptase polymerase chain reaction (RT-PCR). None of the target viruses were detected by one-step PCR. When some of these samples were further examined by two-step PCR, 19.7% (36/183) of spleen sample sets were positive for VHSV, and 4.4% (8/183) of spleen sample sets and 1.2% (3/259) of brain sample sets were positive for NNV. The target sequences of these viruses were clustered with those previously reported in Korea (Genotype IVa of VHSV, RGNNV genotype of NNV) by phylogenetic analysis. The activity of these viruses are not clear because virus isolation was not attempted, but probably very low because all the positive samples were detected by two-step PCR.

Evaluation of Fluoride Removal Effect with Growth of Attached Microbial Community in Middle and Small Stream (중·소하천에서 부착미생물군집의 성장에 따른 불소 제거 효과 평가)

  • Kim, Tae-Kyung;Ryu, Seo-Young;Park, Yoon-A;Lee, Jong-Jun;Joo, Kwang-Jin;Chang, Kwang-Hyeon;Oh, Jong-Min
    • Journal of Environmental Impact Assessment
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    • v.27 no.6
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    • pp.595-603
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    • 2018
  • This study was conducted to understand the growth of attached microbial community in small and medium streams of Gyeonggi-do and the removal efficiency of fluoride with changes in growth. The sites monitoring were carried out for 12 weeks at the P1 and P2(P1 is the point where the discharge water flows. P2 is the downstream point of about 2 km flow), and investigated the water quality and the biomass analysis of the attached microbial community. The growth of the attached microbial community increased up to the 7th investigation, and it was observed that detachment phenomenon occurred. Influencing factors about growth of the attached microbial community were flow rate, velocity, and organic material(T-N & T-P). Meanwhile, fluoride content of attached microbial community also tended to increase until the 7th investigation, and decrease from the 8th. It is assumed that fluoride content has also be reduced with the detachment phenomenon of the attached microbial community. It is expected that this will contribute to the evaluation and management of the use of attached microbial community as a means of stream management. The application of techniques using the attached microbial community should include basic investigation of factors that may affect the growth of the attached microbial community and replacement of the attachment plate according to the time of removal.

Material Characteristics and Ultrasonic Velocity Diagnosis of the Five-storied Stone Pagoda in Tamni-ri, Uiseong (의성 탑리리 오층석탑의 재질특성과 초음파 물성진단)

  • Lee, Myeong Seong;Lee, Jae Man;Kim, Jae Hwan
    • Korean Journal of Heritage: History & Science
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    • v.45 no.1
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    • pp.70-85
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    • 2012
  • Uiseong Tamni-ri Five-storied Stone Pagoda is composed of andesitic tuff and partially combined with tuff breccia and fine-grained granite. The andesitic tuff is identical to basement rock of Geumseongsan Mountain based on lithological, mineralogical and geochemical characteristics. The pagoda has suffered physical weathering such as crack and scaling, discoloration and biological colonization with complex reaction. Expecially, dark gray and brown discoloration appeared whole over the surface of the pagoda, and three to five-layered exfoliation and granular disintegration dominantly occurred in the fourth and fifth roof stones. It is assuming that the stone elements of the pagoda are evaluated as third to forth grades (average third grade) of weathering compared to fresh rock in Geumseongsan Mountain. The physical strength of the stone elements shows low values in the south and west sides of the pagoda that corresponds high weathering degree of the west side due to exfoliation, crack and granular disintegration. It is necessary to investigate the pagoda for precise deterioration assessment, monitoring and conservation treatment.

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.

Analysis of Sequence Type and Fluoroquinolone Resistance in Ciprofloxacin-Resistant Escherichia coli (Ciprofloxacin 내성 대장균에서 Sequence Type과 Fluoroquinolone 내성의 분석)

  • Cho, Hye Hyun
    • Korean Journal of Clinical Laboratory Science
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    • v.53 no.3
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    • pp.217-224
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    • 2021
  • Fluoroquinolone (FQ) resistant gram-negative pathogens have emerged worldwide, and the recent increase in FQ resistant Escherichia coli is of great concern in Korea. This study investigated FQ resistance determinants and the epidemiological relationship of 56 ciprofloxacin-resistant E. coli isolated from a tertiary hospital in Daejeon, South Korea from June to December 2018. Molecular epidemiology was investigated by multilocus sequence typing (MLST). Polymerase chain reaction (PCR) and sequence analysis were performed to identify chromosomal mutations in the quinolone resistance determining regions (QRDR) of gyrA, gyrB, parC, and parE and to describe the occurrence of the following plasmid-mediated quinolone resistance (PMQR) genes: aac(6)-Ib-cr, qepA, qnrA, qnrB, qnrC, qnrD, and qnrS. MLST analysis showed 12 sequence types (STs) and the most prevalent ST was ST131 (31/56, 55.4%), followed by ST1193 (13/56, 23.2%), and ST405 (3/56, 5.4%). In 56 ciprofloxacin-resistant E. coli isolates, Ser83→Leu and Asp87→Asn in gyrA and Ser80→Ile and Glu84→Val in parC (51.8%, 29/56) were the most frequent amino acid substitutions and aac(6)-Ib-cr (33.9%, 19/56) was the most common PMQR gene. These results of FQ resistance determinants were more frequently observed in ST131 compared with other clones. Continuous monitoring of the epidemiological characteristics of ciprofloxacin-resistant E. coli isolates and further investigation of FQ resistance determinants are necessary.