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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 of Analytical Method for Ergot Alkaloids in Foods Using Liquid Chromatoraphy-Tandem Mass Spectrometry (LC-MS/MS를 이용한 식품 중 맥각 알칼로이드 시험법 개발)

  • Chun, So Young;Chong, Euna;Lee, Bomnae;Kwon, Jin-Wook;Park, Hye Young;Kim, Sheenhee;Gang, Giljin
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.158-169
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    • 2019
  • Ergot alkaloids are mycotoxin produced by fungi of the Claviceps genus, mainly by Claviceps purpurea in EU. Recently obtained informations indicates necessity for control the ergot in imported grains. Recent occurrence data of ergot alkaloids from EU countries indicate the necessities of management and control these toxins from the imported grains like rye, wheat, oat etc. The aim of this study is to optimize the liquid chromatography-tandem mass spectrometry method for determination of ergot alkaloids (ergometrine, ergosine, ergotamine, ergocornine, ergocryptine, ergocristine and their epimers (-inines) from grain and grain-based food. The test method was optimized by extracting the sample with acetonitrile containing 2 mM ammonium carbonate, purification with Mycosep cartridge, and instrumental analysis by LC-MS/MS using Syncronis C18 column. The standard calibration curves showed linearity with correlation coefficents; $R^2$ >0.99. Mean recoveries ranged from 72.0 to 111.3% at three different fortified levels (20, 50, and $100{\mu}g/kg$). The correlation coefficient expressed as precision was within the range of 1.9-12.9%. The limit or quantifications (LOQ) ranged from 0.012 to $0.058{\mu}g/kg$. The developed analytical method met the criteria of AOAC Int. and CAC validation parameters like accuracy and sensitivity. As a result, it was confirmed that the test method developed in this study is suitable for the simultaneous analysis of six species of ergot alkaloid from grains and grain products.

Research on an aristocratic officer's travels in the mid Chosun Korea by analysing Yu Hee-chun's diary (일기(日記)를 이용한 조선중기 양반관료의 여행 연구)

  • Jung, Chi-Young
    • Journal of Korean Historical Folklife
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    • no.26
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    • pp.71-106
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    • 2008
  • The objective of this research is to reconstruct an aristocratic officer's travels by analysing Yu, hee-chun's diary, Miamilgi. Yu had kept his diary for eighty three months, from October 1567 to May 1577, and there were twenty six times of travel logs which are analysed in this research. As a result of the analysis, his travels can be divided into official travels and private travels. Sixteen times of official travels were comprised of inspection tours for parishes as a superintendent of Jeonra province, trips to supervise maintenance works of royal tombs and to worship the tombs, to carry out the sanjae (rituals in the mountains) as a second minister of the ministry of rites. It was difficult for him to have private travels as he continually served as a royal officer. He had got only 10 times of private travels during the eighty three months for maintaining the ancestor's tomb and worshiping the ancestors, for recuperating himself and his wife, and for constructing his new house. All of these travels were long-distance ones. In terms of his travel routes, he frequently used royal main trunks, e.g. 'Haenamro' (from Seoul to Damyang), which were maintained by the royal government. The main reason of his frequent using of trunk lines was that convenience facilities such as the royal post stations (Yeok) and royal inns (Won) were equipped well in these roads so it was easy to get horse change services and lodging and boarding. The fact that main trunks were chiefly straight lines and the shortest way was rather secondary reason. On the other hand, when he was a superintendent of Junra province, he had four times of round inspection on all parishes of Junra province, following the tour routs covering all over the province. As he was incumbent royal officer, he started his travel by getting a permission from the king. Simultaneously, he made ready some travel items. Among the items, horse was most important one for the journey. After finishing all the preparing processes before the departure, he had special farewell ceremony for the King, Sookbae, and had a small party with his friends called Jeonbeul. Main transportation means for his travel was horse, and many kinds of horses such as royal government's horse, Yeokma, local government's horse, Swema, as well as his private one were used. Additionally, he used a palanquin while he was doing inspection trip as a superintendent of Junra province. Yu was incumbent officer so he mostly lodged in local government guest houses. If he could not find out any local guest house, he was lodged in royal inn, and in his relatives houses or irregularly in buddhist temples. Most meals were supplied by local royal governments. The activities in his journeys were varied on his travel objectives. In his private journey, it was the main activities that maintaining ancestor's tombs and having a memorial service. During the trip, he visited his relatives. His official trips, on the other hand, had a regularity. Main activities were dealing with public works, and visiting Hyanggyo (country public school). However in the midway, he visited his relatives and had a journey to scenic places.

A Case Study on Introducing Vita Parcours as Forest Leisure Sports Facility in Saneum Healing Forest (산음 치유의 숲 Vita Parcours 도입 사례 연구 - Vita Parcours 도입을 사례로 -)

  • Lee, Jin-Kyu;Kim, Ki Weon
    • The Journal of the Korean Institute of Forest Recreation
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    • v.22 no.4
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    • pp.71-81
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    • 2018
  • It is necessary to build a quality-enhancing forest leisure sports facility according to values that value life quality, national forest policy. Vita Parcours (fitness trails) is found to be the activities highly convenient, so their introduction and promotion in Korea should be highly considered. field survey was necessary to explore the possibility of installing Vita Parcours. Several sites were selected, such as Asean recreational forest, Unaksan recreational forest, Yumyeongsan recreational forest, Saneum recreational forest, Jungmisan recreational forest and National center for forest therapy. At these locations, we explored the current status of forest facilities and forest trails. A total number of 31 exercise facilities has been identified and surveyed, some of which are located on the trails (2), alongside the trail (9), alongside trail boundaries (2) or represent facilities suitable for both outdoor and indoor exercise within the forest (18), all of whom provide location for 44 different exercise routines (flexibility exercises (23), endurance (12) and strength exercises (9)). Field work also included identification of forests paths, the total number of whom was 34 paths - 30 identified as trails, 2 as hiking trails, 1 as a forest path for relaxation and healing and 1 as an exploratory path. Regarding the structure and shape of these trails, 32 was straight in shape and only 2 designed as a circular forest trails. Average length of these trails was 652.2m with the highest and the lowest point altitude difference of 60m, on average. Saneum recreational forest provide the most suitable site/environment for Vita Parcours and as a result of this, Saneum recreational forest is proposed as a location to support the endeavors in promotion of these valuable forest fitness trails. Among the forest paths at this site, a forest path which has a length of 1.84km and 73.0m the highest and the lowest point altitude difference was selected as the most suitable, and may be equipped with necessary stations for exercise or obstacles. In addition, if these trails are to be introduced and welcomed by its users, we must assure that they are properly maintained.

Development and Validation of a Simultaneous Analytical Method for 5 Residual Pesticides in Agricultural Products using GC-MS/MS (GC-MS/MS를 이용한 농산물 중 잔류농약 5종 동시시험법 개발 및 검증)

  • Park, Eun-Ji;Kim, Nam Young;Shim, Jae-Han;Lee, Jung Mi;Jung, Yong Hyun;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.36 no.3
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    • pp.228-238
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    • 2021
  • The aim of this research was to develop a rapid and easy multi-residue method for determining dimethipin, omethoate, dimethipin, chlorfenvinphos and azinphos-methyl in agricultural products (hulled rice, potato, soybean, mandarin and green pepper). Samples were prepared using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and analyzed using gas chromatography-tandem mass spectrometry (GC-MS/MS). Residual pesticides were extracted with 1% acetic acid in acetonitrile followed by addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate. The extracts were cleaned up using MgSO4, primary secondary amine (PSA) and octadecyl (C18). The linearity of the calibration curves, which waas excellent by matrix-matched standards, ranged from 0.005 mg/kg to 0.3 mg/kg and yielded the coefficients of determination (R2) ≥ 0.9934 for all analytes. Average recoveries spiked at three levels (0.01, 0.1, 0.5 mg/kg) and were in the range of 74.2-119.3%, while standard deviation values were less than 14.6%, which is below the Codex guideline (CODEX CAC/GL 40).

Development of simultaneous analytical method for investigation of ketamine and dexmedetomidine in feed (사료 내 케타민과 덱스메데토미딘의 잔류조사를 위한 동시분석법 개발)

  • Chae, Hyun-young;Park, Hyejin;Seo, Hyung-Ju;Jang, Su-nyeong;Lee, Seung Hwa;Jeong, Min-Hee;Cho, Hyunjeong;Hong, Seong-Hee;Na, Tae Woong
    • Analytical Science and Technology
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    • v.35 no.3
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    • pp.136-142
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    • 2022
  • According to media reports, the carcasses of euthanized abandoned dogs were processed at high temperature and pressure to make powder, and then used as feed materials (meat and bone meal), raising the possibility of residuals in the feed of the anesthetic ketamine and dexmedetomidine used for euthanasia. Therefore, a simultaneous analysis method using QuEChERS combined with high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry was developed for rapid residue analysis. The method developed in this study exhibited linearity of 0.999 and higher. Selectivity was evaluated by analyzing blank and spiked samples at the limit of quantification. The MRM chromatograms of blank samples were compared with those of spiked samples with the analyte, and there were no interferences at the respective retention times of ketamine and dexmedetomidine. The detection and quantitation limits of the instrument were 0.6 ㎍/L and 2 ㎍/L, respectively. The limit of quantitation for the method was 10 ㎍/kg. The results of the recovery test on meat and bone meal, meat meal, and pet food showed ketamine in the range of 80.48-98.63 % with less than 5.00 % RSD, and dexmedetomidine in the range of 72.75-93.00 % with less than 4.83 % RSD. As a result of collecting and analyzing six feeds, such as meat and bone meal, prepared at the time the raw material was distributed, 10.8 ㎍/kg of ketamine was detected in one sample of meat and bone meal, while dexmedetomidine was found to have a concentration below the limit of quantitation. It was confirmed that the detected sample was distributed before the safety issue was known, and thereafter, all the meat and bone meal made with the carcasses of euthanized abandoned dogs was recalled and completely discarded. To ensure the safety of the meat and bone meal, 32 samples of the meat and bone meal as well as compound feed were collected, and additional residue investigations were conducted for ketamine and dexmedetomidine. As a result of the analysis, no component was detected. However, through this investigation, it was confirmed that some animal drugs, such as anesthetics, can remain without decomposition even at high temperature and pressure; therefore, there is a need for further investigation of other potentially hazardous substances not controlled in the feed.

Root and Canal Morphology of Maxillary Primary Molar using CBCT and 3D CT (CBCT 및 3D CT를 활용한 상악 유구치 치근과 근관 형태)

  • Kim, Joon Hee;Kim, Hyuntae;Shin, Teo Jeon;Hyun, Hong-Keun;Kim, Young-Jae;Kim, Jung-Wook;Jang, Ki-Taeg;Song, Ji-Soo
    • Journal of the korean academy of Pediatric Dentistry
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    • v.48 no.4
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    • pp.437-448
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    • 2021
  • The purpose of this study is to analyze morphological characteristics of maxillary primary molar's root and root canal. 268 children aged 3 - 7 years (175 boys, 93 girls) who had CBCT (152 children) and 3D CT (116 children) taken in Seoul National University Dental Hospital from January 2006 to April 2020 were included. The number of roots and root canals were analyzed in 1002 teeth without any root resorption or periapical pathologies. Curvature, angulation, length of root and root canal, as well as cross-sectional shapes of the root canal were analyzed in 218 teeth. By using Mimics and 3-Matics software, volume, surface area, and volume ratio of root canal was analyzed in 48 teeth. More than half of maxillary primary molars have 3 roots and 3 root canals. The degree of symmetry of root canal type was about 0.63 (Cohen's kappa coefficient). The most frequent shape of roots and canals was linear in 1st primary molars and curved in 2nd primary molars. Angulation, length of root and root canals was the largest on palatal roots. Most teeth showed ovoid or round shapes at apex. The largest root canal volume, surface area, volume ratio was found in the palatal roots.

Simultaneous determinations of anthracycline antibiotics by high performance liquid chromatography coupled with radial-flow electrochemical cell (고성능 액체 크로마토그래피/방사흐름 전기화학전지를 이용한 안트라사이클린계 항생제의 동시 정량)

  • Cho, Yonghee;Hahn, Younghee
    • Analytical Science and Technology
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    • v.20 no.4
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    • pp.308-314
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    • 2007
  • The analytical method of HPLC with the radial-flow electrochemical cell (RFEC) has been developed to determine doxorubicin, epirubicin, nogalamycin, daunorubicin and idarubicin simultaneously by employing a reversed-phase chromatography. Anthracyclines were detected at -0.74 V vs. a Ag/AgCl (0.01 M NaCl) reference electrode, a potential of diffusion current plateau in the mobile phase. At a $V_f$ of 1.0 mL/min doxorubicin, epirubicin, daunorubicin and idarubicin appeared at a retention time ($t_r$) of 6.4 min, 7.4 min, 12.7 min and 18.4 min, respectively, while at a $V_f$ of 0.6 mL/min, doxorubicin, epirubicin, nogalamycin, daunorubicin and idarubicin appeared at a $t_r$ of 9.9 min, 11.5 min, 13.5 min, 19.6 min and 28.7 min, respectively. The linearity between each anthracycline injected ($2.40{\times}10^{-7}M{\sim}1.42{\times}10^{-5}M$) and peak area (charge) was excellent with the square of the correlation coefficient ($R^2$) higher than 0.999. The detection limits were $1.0{\times}10^{-8}M{\sim}1.5{\times}10^{-7}M$ for the five anthracyclines. Within-day precision for the five anthracyclines were in reasonable relative standard deviations less than 3 % ($1.00{\times}10^{-6}M{\sim}1.42{\times}10^{-5}M$) except the lower concentrations less than $0.7{\mu}M$. Solid phase extractions of $1.00{\times}10^{-5}M$ epirubicin, $0.48{\times}10^{-5}M$ nogalamycin and $1.52{\times}10^{-5}M$ daunorubicin from human serum with a $C_{18}$ cartridge resulted in 97 %, 100 % and 90 % of recoveries, respectively.

A study of analytical method for Benzo[a]pyrene in edible oils (식용유지 중 벤조피렌 분석법 비교 연구)

  • Min-Jeong Kim;jun-Young Park;Min-Ju Kim;Eun-Young Jo;Mi-Young Park;Nan-Sook Han;Sook-Nam Hwang
    • Analytical Science and Technology
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    • v.36 no.6
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    • pp.291-299
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    • 2023
  • The benzo[a]pyrene in edible oils is extracted using methods such as Liquid-liquid, soxhlet and ultrasound-assisted extraction. However these extraction methods have significant drawbacks, such as long extraction time and large amount of solvent usage. To overcome these drawbacks, this study attempted to improve the current complex benzo[a]pyrene analysis method by applying the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method that can be analyzed in a simple and short time. The QuEChERS method applied in this study includes extraction of benzo[a]pyrene into n-hexane saturated acetonitrile and n-hexane. After extraction and distribution using magnesium sulfate and sodium chloride, benzo[a]pyrene is analyzed by liquid chromatography with fluorescence detector (LC/FLR). As a result of method validation of the new method, the limit of detection (LOD) and quantification (LOQ) were 0.02 ㎍/kg and 0.05 ㎍/kg, respectively. The calibration curves were constructed using five levels (0.1~10 ㎍/kg) and coefficient (R2) was above 0.99. Mean recovery ratio was ranged from 74.5 to 79.3 % with a relative standard deviation (RSD) between 0.52 to 1.58 %. The accuracy and precision were 72.6~79.4 % and 0.14~7.20 %, respectively. All results satisfied the criteria ranges requested in the Food Safety Evaluation Department guidelines (2016) and AOAC official method of analysis (2023). Therefore, the analysis method presented in this study was a relatively simple pretreatment method compared to the existing analysis method, which reduced the analysis time and solvent use to 92 % and 96 %, respectively.

Development of a Simultaneous Analytical Method for Azocyclotin, Cyhexatin, and Fenbutatin Oxide Detection in Livestock Products using the LC-MS/MS (LC-MS/MS를 이용한 축산물 중 유기주석계 농약 Azocyclotin, Cyhexatin 및 Fenbutatin oxide의 동시시험법 개발)

  • Nam Young Kim;Eun-Ji Park;So-Ra Park;Jung Mi Lee;Yong Hyun Jung;Hae Jung Yoon
    • Journal of Food Hygiene and Safety
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    • v.38 no.5
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    • pp.361-372
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    • 2023
  • Organotin pesticide is used as an acaricide in agriculture and may contaminate livestock products. This study aims to develop a rapid and straightforward analytical method for detecting organotin pesticides, specifically azocyclotin, cyhexatin, and fenbutatin oxide, in various livestock products, including beef, pork, chicken, egg, and milk, using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The extraction process involved the use of 1% acetic acid in a mixture of acetonitrile and ethyl acetate (1:1). This was followed by the addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium chloride. The extracts were subsequently purified using octadecyl (C18) and primary secondary amine (PSA), after which the supernatant was evaporated. Organotin pesticide recovery ranged from 75.7 to 115.3%, with a coefficient of variation (CV) below 25.3%. The results meet the criteria range of the Codex guidelines (CODEX CAC/GL 40). The analytical method in this study will be invaluable for the analysis of organotin pesticides in livestock products.