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Development and Validation of an Analytical Method for Quinoxyfen in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 살균제 Quinoxyfen의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.140-147
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    • 2019
  • An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

Development and Validation of an Analytical Method for Fenpropimorph in Agricultural Products Using QuEChERS and LC-MS/MS (QuEChERS법과 LC-MS/MS를 이용한 농산물 중 Fenpropimorph 시험법 개발 및 검증)

  • Lee, Han Sol;Do, Jung-Ah;Park, Ji-Su;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.115-123
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    • 2019
  • An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.

Determination and Validation of an Analytical Method for Dichlobentiazox in Agricultural Products with LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Dichlobentiazox 시험법 개발 및 검증)

  • Gu, Sun Young;Lee, Han Sol;Park, Ji-Su;Lee, Su Jung;Shin, Hye-Sun;Kang, Sung Eun;Chung, Yun Mi;Choi, Ha Na;Yoon, Sang Soon;Jung, Young-Hyun;Yoon, Hae Jung
    • Korean Journal of Environmental Agriculture
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    • v.40 no.2
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    • pp.108-117
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    • 2021
  • BACKGROUND: Dichlobentiazox is a newly registered pesticide in Korea as a triazole fungicide and requires establishment of an official analysis method for the safety management. Therefore, the aim of this study was to determine the residual analysis method of dichlobentiazox for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods were applied to establish the extraction method, and the EN method was finally selected through the recovery test. In addition, various adsorbent agents were applied to establish the clean-up method. As a result, it was found that the recovery of the tested pesticide was reduced when using the d-SPE method with PSA and GCB, but C18 showed an excellent recovery. Therefore this method was established as the final analysis method. For the analysis, LC-MS/MS was used with consideration of the selectivity and sensitivity of the target pesticide and was operated in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 70-120%, with standard deviation and coefficient of variation of less than 3.0% and 11.6%, respectively. CONCLUSION: Dichlobentiazox could be analyzed with a modified QuEChERS method, and the method determined would be widely available to ensure the safety of residual pesticides in Korea.

Evaluations of Growth and Forage Quality of Sesbania Accessions Adaptable to Korean Environments (국내적응 세스바니아의 생육특성 및 사료가치 평가)

  • Lee, Chang Min;Kim, Young Jin;Ahn, Sol;Hailegioris, Daniel;Lee, Cheong Ae;Yun, Song-Joong
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.64 no.3
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    • pp.278-286
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    • 2019
  • Sesbania, an annual herb, is known for its high forage value and salt tolerance. It has merits as a forage crop that is adaptable to reclaimed land in the Republic of Korea. Therefore, we collected Sesbania genetic resources from the Republic of Korea and other countries, and conducted experiments to evaluate their potential as a forage crop in Korean climate and soil conditions. In the preliminary experiments, 15 genetic resources which were able to set seeds in Korean environment were selected out of a total of 46 collected genetic resources. Among 15 genetic resources, SL13 was the tallest and it was followed by that of SC04, SR01 and SE07. The accessions with the earliest flowering started flowering 101 days after sowing and set seed in early August. Fifteen accessions were evaluated for their salt tolerance at germination stage based on germination rate and growth of germinated seedlings at 0 mM, 150 mM and 300 mM NaCl concentrations. Five genetic resources like SC04, SL13, SS20, SS24 and SR01 were selected to be tolerant to NaCl treatment. Forage value was evaluated based on crude protein, acid detergent fiber, neutral detergent fiber and in vitro dry matter digestibility. The forage value of leaves was significantly higher than that of stems, and the forage value of the stem was slightly better than that of rice straw. The forage value of leaves of all the genetic resources was higher than grade 1 by the American Forage and Grassland Council grade. Among five selected genetic resources, the relative feed value of SC04 was the highest and it was followed by that of SS20, SL13, SS24 and SR01.

The Detection and Density Fluctuation of Mulberry Dwarf Phytoplasma using Nested-PCR and Competitive-PCR Methods (Nested-PCR법과 Competitive PCR법을 이용한 뽕나무 오갈병(MD) Phytoplasma의 검출과 밀도변화)

  • Chae, Seungmin;Lee, Sol;Cha, Byeongjin;Lee, Hyokin;Han, Sangsub
    • Journal of Korean Society of Forest Science
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    • v.100 no.4
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    • pp.623-629
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    • 2011
  • The detectable levels and population fluctuations of phytoplasmas infecting dwarf mulberry trees were investigated using nested-PCR and competitive-PCR methods. Samples of five different types were studied : A. petiole of a leaf that displays dwarf symptoms, B. petiole from apparently healthy leaf residing on a branch also supports a leaf with dwarf symptoms, C. the branch portion that supports a leaf with dwarf symptoms, D. the leaf petiole from healthy appearing leaves on branch with no dwarf symptoms, and branch portion of branch with no dwarf symptoms, E. the rootlets of trees with dwarf symptoms. These 5-parts were collected from each tree during June - April, once in every two months. The phytoplasma was detected from all parts of collected mulberry samples during all seasons using nested-PCR with AS-1/AS-2 primer pairs. The phytoplasma was detected until $10^4$ dilution using direct-PCR method, but it was detected until $10^{13}$ dilution by the nested-PCR method. The density of pytoplasma was found to be $7.94{\times}10^{18}-10^{12}copies/{\mu}L$ in mulberry trees. The density of phytoplasma was observed throughout the year in all samples of mulberry trees. The highest rates of phytoplasma was found in the samples B and C during the early growing season followed by the sample A and D during the dormant season. Samples C and E displayed the highest phytoplasma density followed sample D. The density of phytoplasma appeared stable during all the seasons for samples C and A. The result of the present study demonstrates the utility of nested-PCR and competitive-PCR for detection and determination of population fluctuations of phytoplasmas in plant tissues.

1H Solid-state NMR Methodology Study for the Quantification of Water Content of Amorphous Silica Nanoparticles Depending on Relative Humidity (상대습도에 따른 비정질 규산염 나노입자의 함수량 정량 분석을 위한 1H 고상 핵자기 공명 분광분석 방법론 연구)

  • Oh, Sol Bi;Kim, Hyun Na
    • Korean Journal of Mineralogy and Petrology
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    • v.34 no.1
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    • pp.31-40
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    • 2021
  • The hydrogen in nominally anhydrous mineral is known to be associated with lattice defects, but it also can exist in the form of water and hydroxyl groups on the large surface of the nanoscale particles. In this study, we investigate the effectiveness of 1H solid-state nuclear magnetic resonance (NMR) spectroscopy as a robust experimental method to quantify the hydrogen atomic environments of amorphous silica nanoparticles with varying relative humidity. Amorphous silica nanoparticles were packed into NMR rotors in a temperature-humidity controlled glove box, then stored in different atmospheric conditions with 25% and 70% relative humidity for 2~10 days until 1H NMR experiments, and a slight difference was observed in 1H NMR spectra. These results indicate that amount of hydrous species in the sample packed in the NMR rotor is rarely changed by the external atmosphere. The amount of hydrogen atom, especially the amount of physisorbed water may vary in the range of ~10% due to the temporal and spatial inhomogeneity of relative humidity in the glove box. The quantitative analysis of 1H NMR spectra shows that the amount of hydrogen atom in amorphous silica nanoparticles linearly increases as the relative humidity increases. These results imply that the sample sealing capability of the NMR rotor is sufficient to preserve the hydrous environments of samples, and is suitable for the quantitative measurement of water content of ultrafine nominally anhydrous minerals depending on the atmospheric relative humidity. We expect that 1H solid-state NMR method is suitable to investigate systematically the effect of surface area and crystallinity on the water content of diverse nano-sized nominally anhydrous minerals with varying relative humidity.

The control of TiO2 nanofiber diameters using fabrication variables in electrospinning method (전기 방사 공정의 제조 변수를 이용한 TiO2 나노섬유의 직경 제어)

  • Yoon, Han-Sol;Kim, Bo-Sung;Kim, Wan-Tae;Na, Kyeong-Han;Lee, Jung-Woo;Yang, Wan-Hee;Park, Dong-Cheol;Choi, Won-Youl
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.31 no.1
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    • pp.8-15
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    • 2021
  • TiO2 has been used in various fields such as solar cells, dental implants, and photocatalysis, because it has high physical and chemical stability and is harmless to the body. TiO2 nanofibers which have a large specific surface area also show a good reactivity in bio-friendly products and excellent photocatalysis in air and water purification. To fabricate TiO2 nanofibers, an electrospinning method was used. To observe the diameter of TiO2 nanofibers with fabrication variables, the fabrication variables was divided into precursor composition variables and process variables and microstructure was analyzed. The concentrations of PVP (Polyvinylpyrrolidone) and TTIP (Titanium(IV) isopropoxide) were selected as precursor composition variables, and inflow velocity and voltage were also selected as process variables. Microstructure and crystal structure of TiO2 nanofibers were analyzed using FE-SEM (Field emission scanning electron microscope) and XRD (X-ray diffraction), respectively. As-spun TiO2 nanofibers with an average diameter of about 0.27 ㎛ to 1.31 ㎛ were transformed to anatase TiO2 nanofibers with an average diameter of about 0.22 ㎛ to 0.78 ㎛ after heat treatment of 3 hours at 450℃. Anatase TiO2 nanofibers with an average diameter of 0.22 ㎛ can be expected to improve the photocatalytic properties by increasing the specific surface area. To change the average diameter of TiO2 nanofibers, the control of precursor composition variables such as concentrations of PVP and TTIP is more efficient than the control of electrospinning process variables such as inflow velocity and voltage.

Report on the improvement of the in vitro and specimen reception environment system (핵의학과 검체 접수 환경시스템의 개선사례 보고)

  • Kim, Jung In;Kang, Mi Ji;Kim, Na Kyung;Park, Ji Sol;Kwon, Won Hyun;Lee, Kyung Jae
    • The Korean Journal of Nuclear Medicine Technology
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    • v.25 no.2
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    • pp.29-34
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    • 2021
  • Purpose Sample reception environment system in nuclear medicine has not changed much compared to 20 years ago. When preparing sample for in vitro test, there was no significant change because the test was carried out by generating an own specimen from the parent specimen. In this study, We would like to introduce a method that automatically removes the sample cap using the automated decapper equipment and enables automatic reception at the same time. In addition, including a provisional reception system. Materials and Methods In 2019, it was intended to get a device that automatically removes the cap of a patient's blood sample. This equipment is the same as the equipment used in the Department of Laboratory Medicine (Vacuette Ⓡ Unicap Belt Decapper, Greiner bio-one, Austria). However, the purchase was delayed due to differences in tube size, budget, and space. In January 2020, we borrowed domestic automatic decapper equipment and modified it to suit our laboratory environment. After 9 months, we were able to introduce a system that automatically removes the lid of a patient's blood sample and at the same time automatically accepts the test. And, through the provisional reception system, it was possible to know the arrival of the specimen in a short time. Results With the use of an automatic decapper device, the sample cap was automatically removed, and the reception proceeded at the same time. So, it was very efficient at work because it shortened the sample preparation time by about 20 minutes. In addition, it was possible to prevent the examiner's musculoskeletal disorders caused by repeated wrist use. After using the provisional reception system, patients were able to be discharged quickly, and the number of phone calls to confirm the arrival of samples was reduced. Conclusion Most hospitals have about four employees in the nuclear medicine in vitro laboratory. It is effective to use automatic decapper equipment and a provisional reception system for organizations that perform work with the minimum number of personnel.

Investigation of microbial contamination on manufacturing processes for small-scale Korean traditional cookies manufacturers (소규모 한과제조업체의 제조공정에 대한 미생물 오염 조사)

  • Kim Sol-A;Lee, Jeong-Eun;Park, Hyun-Jin;Park, Mi-Seon;Choi, Song Yi;Shim, Won-Bo
    • Journal of Food Hygiene and Safety
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    • v.36 no.6
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    • pp.493-503
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    • 2021
  • The study was designed to analyze raw and auxiliary materials of Korean traditional cookies such as Yugwa and Gangjeong, equipment and tools, personal hygiene of workers and microbial contamination of materials by each manufacturing process. In addition, it looked at washing method for reducing microorganisms at the site and reduction effect of microorganisms by frequency in the manufacturing processes of Yugwa. In the process of producing Korean traditional cookies, the level of total aerobic bacteria (TAB) in popped rice was 1.2 Log CFU/g and the level of TAB in finished products increased to 3.7 Log CFU/g. In the process of producing Yugwa, the level of TAB increased to a maximum of 6.5 Log CFU/g in the soaking process but decreased to 1.3 Log CFU/g in the frying process. However, the level of TAB increased again to 1.3 Log CFU/g in finished products that proves its recontamination. It is estimated that he manufacturing process causes cross-contamination that comes from the work tools, equipment or workers. In particular, the spatula, one of the work tools, was found to have 4.4 Log CFU/g of aerobic bacteria and 4.2 Log CFU/g of colon bacillus that show they are highly contaminated. In the soaking process of Yugwa that lasts seven days, the level of TAB was a maximum of 10 Log CFU/g and the level of total colon bacillus was 6.8 Log CFU/g. When compared with washing methods, using hands and tools or running water, it is confirmed that the level of both TAB and total colon bacillus decreased to 5.0 Log CFU/g and 2.8 Log CFU/g respectively when hands were washed with running water 10 times. The above result shows that it's required for workers to wash their hands as well as wash and disinfect work tools and equipment in the process of producing Korean traditional cookies at small-scale companies. In addition, to reduce the level of microbial contamination in finished products, workers are required to apply their reduction method at the site.

Evaluation of the usefulness of the method according to changes in patient breathing during chest 4D CT imaging (흉부 4D CT에서 호흡 변화에 대한 일시 중지 및 재개 방법의 유용성 평가)

  • Heo, Sol;Shin, Chung Hun;Jeong, Hyun Sook;Yoo, Soon Mi;Kim, Jeong Mi;Yun, In Ha;Hong, Seung Mo;Back, Geum Mun
    • The Journal of Korean Society for Radiation Therapy
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    • v.33
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    • pp.47-54
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    • 2021
  • Purpose : In order to evaluate the usefulness of clinical application of the Pause & Resume methods by comparing and analyzing the data stability and dose reduction effect when repeat scan assuming irregular breathing and using the Pause & Resume method during chest 4D CT using QuasarTM Phantom. Materials and Methods : Using the QuasarTM Phantom, set the breathing rate per minute to 15 BPM and 7.5 BPM, and set the S15 point as an irregular breathing section, and then placed OSLD to this point and use the Pause & Resume method to measure the dose of S15. CTDIvol, DLP, and ALARA-CT were used for comparative analysis of radiation dose between Pause & Resume method and Repeat-scan. In order to evaluate the stability and usability of the data applying the Pause & Resume method, the captured images were sorted by Advanced Workstation Volume Share7 and then sent to EclipseTM, the diameter and volume were analyzed by forming a contour on the iron ball in the QuasarTM Phantom Results : When using Pause & Resume, the dose of OSLD measurement increased by 1.97 times in the section of S15. As a result of image evaluation, the average value of all volumes measured with and without the Pause & Resume method at 15 BPM and 7.5 BPM was 15.2 cm3±0.5%.Allthemeasuredvaluesfor the radius of iron ball were 3.1 cm regardless of whether Pause & Resume method was used or not. In the case of using Pause & Resume, 33% decreased from the lowest DLP value and 38% decreased from the highest DLP value of repeat scan, and the effective dose also decreased 32.1% from the minimum value and 37.6% from the maximum value. Conclusion: Irradiation dose was increased by Pause & Resume method because of the repeat scan on the S15 site where assuming irregular breathing occurred, However Pause & Resume method led to a significant reduction in dose on overall scan range. It also proved the usefulness of clinical application of the Pause & Resume method as a result of similar diameters and volumes of iron ball measurement.