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Development of an Official Analytical Method for Determination of Imazapyr in Agricultural Commodities using HPLC-UVD (HPLC-UVD를 이용한 농산물 중 Imazapyr의 공정분석법 확립)

  • Jang, Jin;Kim, Heejung;Ko, Ah-Young;Lee, Eun-Hyang;Joo, Yoon Ji;Kim, Jinhong;Chang, Moon-Ik;Rhee, Gyu-Seek
    • The Korean Journal of Pesticide Science
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    • v.19 no.1
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    • pp.5-13
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    • 2015
  • A chromatographic method for the determination of imazapyr, a non-selective herbicide, in agricultural commodities was developed to use safety control of pesticide residue on crops, and was fully validated as an official method for residue analysis. Agricultural commodities, mandarin (fruit), hulled rice (cereal grains), pepper (vegetables), potato (potatoes) and soybean (beans) were extracted with methanol and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2.5 by 4N hydrochloric acid. Finally, they were analyzed by high performance liquid chromatography coupled to UV detector (HPLC-UVD). The developed method had the linearity in the range of test concentrations with coefficients of determination ($r^2$) more than 0.99. Recovery studies were carried out at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. Recoveries were ranged between 72.1 to 108.0%, with relative standard deviations less than 10%. A consistent recovery was determined according to the CODEX guidelines (CAC/GL40, 2003). Finally, LC/MS with selected ion monitoring was also applied to confirm the suspected residues of imazapyr in agricultural samples. This developed method for determination of imazapyr residues in agricultural commodities. can be used as an official method.

Estimation of Fresh Weight and Leaf Area Index of Soybean (Glycine max) Using Multi-year Spectral Data (다년도 분광 데이터를 이용한 콩의 생체중, 엽면적 지수 추정)

  • Jang, Si-Hyeong;Ryu, Chan-Seok;Kang, Ye-Seong;Park, Jun-Woo;Kim, Tae-Yang;Kang, Kyung-Suk;Park, Min-Jun;Baek, Hyun-Chan;Park, Yu-hyeon;Kang, Dong-woo;Zou, Kunyan;Kim, Min-Cheol;Kwon, Yeon-Ju;Han, Seung-ah;Jun, Tae-Hwan
    • Korean Journal of Agricultural and Forest Meteorology
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    • v.23 no.4
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    • pp.329-339
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    • 2021
  • Soybeans (Glycine max), one of major upland crops, require precise management of environmental conditions, such as temperature, water, and soil, during cultivation since they are sensitive to environmental changes. Application of spectral technologies that measure the physiological state of crops remotely has great potential for improving quality and productivity of the soybean by estimating yields, physiological stresses, and diseases. In this study, we developed and validated a soybean growth prediction model using multispectral imagery. We conducted a linear regression analysis between vegetation indices and soybean growth data (fresh weight and LAI) obtained at Miryang fields. The linear regression model was validated at Goesan fields. It was found that the model based on green ratio vegetation index (GRVI) had the greatest performance in prediction of fresh weight at the calibration stage (R2=0.74, RMSE=246 g/m2, RE=34.2%). In the validation stage, RMSE and RE of the model were 392 g/m2 and 32%, respectively. The errors of the model differed by cropping system, For example, RMSE and RE of model in single crop fields were 315 g/m2 and 26%, respectively. On the other hand, the model had greater values of RMSE (381 g/m2) and RE (31%) in double crop fields. As a result of developing models for predicting a fresh weight into two years (2018+2020) with similar accumulated temperature (AT) in three years and a single year (2019) that was different from that AT, the prediction performance of a single year model was better than a two years model. Consequently, compared with those models divided by AT and a three years model, RMSE of a single crop fields were improved by about 29.1%. However, those of double crop fields decreased by about 19.6%. When environmental factors are used along with, spectral data, the reliability of soybean growth prediction can be achieved various environmental conditions.

Development and Validation of Analytical Method for Determination of Fungicide Spiroxamine Residue in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Spiroxamine의 시험법 개발 및 검증)

  • Park, Shin-Min;Do, Jung-Ah;Lim, Seung-Hee;Yoon, Ji-Hye;Pak, Won-Min;Shin, Hye-Sun;Kuk, Ju-Hee;Chung, Hyung-Wook
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.296-305
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    • 2018
  • Spiroxamine, one of fungicides, is used to control powdery mildew in various crops and black yellow sigatoka in bananas. The major strength of spiroxamine is to control powdery mildew in various crops and bananas yellow sigatoka in bananas. The compound has shown a high level of activity, good persistence and crop tolerance. Besides powdery mildew, good control of rust, net blotch and Rhynchosporium diseases been indicated in cereals, together with a complementary activity against Septoria diseases. In 2017, the maximum residue limit (MRL) of spiroxamine established in Korea. According to Ministry of ood and rug afety) regulations, spiroxamine residues defined only parent compound. Thus, a analytical method is needed to estimate the residue level of the parent compound. The objective of this study was to develop and validate analytical method for spiroxamine in representative agricultural commodities. Samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interfering substances. The analyte were quantified and confirmed liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive-ion mode using multiple reaction monitoring (MRM). Matrix matched calibration curves were linear over the calibration ranges ($0.0005{\sim}0.1{\mu}g/mL$) for the analyte in blank extract with coefficient of determination ($r^2$) > 0.99. For validation purposes, recovery studies will be carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries 70.6~104.6% with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges in the Codex guidelines (CAC/GL40, 2003) and MFDS guidelines. proposed analytical method be used as an official analytical method in the Republic of Korea.

The Partitioning Characteristics of Heavy Metals in Soils of Ulsan by Sequential Extraction Procedures (단계별추출법에 의한 울산지역 토양 중의 중금속 Partitioning 특성연구)

  • Lee, Byeong-Kyu;Koh, Il-Ha;Kim, Haeng-Ah
    • Journal of Korean Society of Environmental Engineers
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    • v.27 no.1
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    • pp.25-35
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    • 2005
  • This study analyzed total concentrations and existing forms of heavy metals in soils of Ulsan using a sequential extraction method. Soil samples were collected from 6 categorized areas including green, residential, heavy traffic, petrochemical industrial complex(IC), mechanical and shipbuilding IC, and non-ferrous metal IC areas. which represent different emission characteristics. The highest total concentrations of heavy metals by a sequential extraction analysis were observed in the soils collected from the non-ferrous metal IC area, followed by the mechanical and shipbuilding IC and heavy traffic areas. Dominant(> 50%) existing forms of Cd, Cr and Ni were residual forms followed by Fe and Mn oxides in almost areas. Residual fractions in the non-ferrous metal IC areas were relatively lower than those in other areas. However, the fractions of organic and sulphides in the IC areas were higher. The dominant farms of Cu were much different with the investigated areas. In most areas, the dominant forms of Pb and Zn were Fe and Mn oxides, followed by residual fraction for Pb. The exchangeable and carbonate fractions represent mobility of metallic elements in soils. They are also significantly affected by the environmental renditions, such as pHs of soil and rainfall. In this study the exchangeable and carbonate fractions were lower than other fractions. Because the total concentrations of heavy metals in the soils of the non-ferrous metal IC area were extremely high, however, the mobile fractions of heavy metals in the IC area would be significant. Thus a large amount of heavy metals can be released into plants, water bodies, and soils. Therefore, urgent measures, such as source control for soil remediation of heavy metals, in the non-ferrous metal IC areas are essentially required. Analysis results obtained from the sequential extraction and the aqua regia extraction showed a high correlation, whose determination coefficients(R2) of heavy metals except Cd approximately ranged from 0.7 to 0.9.

A Study on Total Mercury and Methylmercury in Commercial Tuna, Billfish, and Deep-sea Fish in Seoul Metropolitan City (서울시 유통 다랑어류, 새치류 및 심해성 어류의 총수은 및 메틸수은 축적에 대한 고찰)

  • Kim, Jin-Ah;Yuk, Dong-Hyun;Park, Young-Ae;Choi, Hee-Jin;Kim, Youn-Cheon;Kim, Moo-Sang
    • Korean Journal of Food Science and Technology
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    • v.45 no.3
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    • pp.376-381
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    • 2013
  • In this study, we monitored total mercury and methylmercury concentrations in tuna, billfish, and deep-sea fish distributed in Seoul city. With the acquired data, we carried out statistical analysis and an exposure assessment for intake. The mean concentrations (mg/kg) of total mercury and methylmercury were $0.32{\pm}0.31/0.20{\pm}0.20$ for tuna, $0.43{\pm}0.48/0.20{\pm}0.17$ for patagonian toothfish, $0.99{\pm}0.72/0.51{\pm}0.40$ for billfish and $1.20{\pm}0.70/0.95{\pm}0.51$ for sharks, respectively. We found that sharks, billfish, patagonian toothfish, and tuna were more contaminated with total mercury and methylmercury, in sequence, and that 66% of the total mercury concentration consisted of methylmercury, on average. Although the estimated weekly intakes of methylmercury from commercial deep-sea fish were lower than the weekly intakes recommended by the Joint FAO/WHO Expert Committee on Food Additives (JECFA), we identified that the total mercury and methylmercury concentrations in tuna, billfish, and deep-sea fish continued to increase with the passage of time. Therefore, we confirmed the necessity of continuous monitoring and comprehensive analysis for general safety.

Development and Validation of an Analytical Method for Fungicide Sedaxane Determination in Agricultural Products using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Sedaxane의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Park, Shin-Min;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.1
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    • pp.30-39
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    • 2019
  • An analytical method was developed for the determination of sedaxane in agricultural products using liquid chromatograph-tandem mass spectrometry (LC-MS/MS). The samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, and then purified by using silica SPE cartridges to clean up. The analytes were quantified and confirmed by using LC-MS/MS in positive ion mode using multiple reaction monitoring (MRM). The matrix-matched calibration curves were linear over the calibration ranges ($0.001-0.25{\mu}g/mL$) into a blank extract with $r^2$>0.99. For validation, recovery tests were carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ, n=5) with five replicates performed at each level. The recoveries were ranged between 74.5 to 100.8% with relative standard deviations (RSDs) of less than 12.1% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for sedaxane determination in agricultural commodities.

Analysis of newborn hearing screening using automated auditory brainstem response (자동화 청성뇌간반응을 이용한 신생아 청력선별검사 결과 분석)

  • Park, Sung Won;Yun, Byung Ho;Kim, Kyung Ah;Ko, Sun Young;Lee, Yeon Kyung;Shin, Son Moon;Hong, Sung Hwa
    • Clinical and Experimental Pediatrics
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    • v.49 no.10
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    • pp.1056-1060
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    • 2006
  • Purpose : As hearing ability affects language and cognitive development, early detection and intervention of congenital hearing defects is very important. We analyzed the result of newborn hearing screening using automated auditory brainstem response and estimated the incidence of congenital hearing defects in newborn infants in Korea. Methods : Hearing screening tests were done on 7,218 newborn infants who were delivered at Cheil General Hospital from July 1, 2004 to June 30, 2005. The first screening test was done on the second day of life with automated auditory brainstem response(AABR) using $ALGO{\bigcirc}^{(3)}$ Newborn hearing screener($Natus^{(R)}$ Medical Incorporated, San Carlos, USA) with 35 dB sound level. The newborn infants who did not pass the initial screening test took the second screening AABR test before discharge from the nursery. Infants who did not pass these screenings at the nursery were followed up at the Department of Otorhinolaryngology, Samsung Seoul Hospital. Results : Total 7,218 infants(83.3 percent of total 8,664 live births of the Cheil General Hospital) were screened in the nursery, and 55 of them failed to pass the newborn screening. Among 55 infants who were referred, six were lost during follow-up, and 14 were confirmed as hearing impaired. Six of them(42.8 percent) do not have any risk factors for hearing impairment. We can estimate that the incidence of hearing defects is about 1.9-2.8 per 1,000 live births. Conclusion : Automated auditory brainstem response is an effective tool to screen the hearing of newborn infants. Congenital hearing loss is more frequent than metabolic diseases on which screening tests are available in the newborn period. About 40 percent of infants who have hearing defects do not have any risk factors for hearing impairment. Therefore, universal newborn hearing screening must be recommended to all neonates.

The Differentiation of Malignant and Benign Musculoskeletal Tumors by F-18 FDG PET/CT Studies - Determination of maxSUV by Analysis of ROC Curve (F-18 FDG PET/CT에서 양성과 악성 근골격 종양의 감별진단 - 수신자 판단특성곡선을 이용한 maxSUV의 절단값 결정)

  • Kong, Eun-Jung;Cho, Ihn-Ho;Chun, Kyung-Ah;Won, Kyu-Chang;Lee, Hyung-Woo;Choi, Jun-Heok;Shin, Duk-Seop
    • Nuclear Medicine and Molecular Imaging
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    • v.41 no.6
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    • pp.553-560
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    • 2007
  • Purpose: We evaluated the standard uptake value (SUV) of F-18 FDG at PET/CT for differentiation of benign from malignant tumor in primary musculoskeletal tumors. Materials and Methods: Forty-six tumors (11 benign and 12 malignant soft tissue tumors, 9 benign and 14 malignant bone tumors) were examined with F-18 FDG PET/CT (Discovery ST, GE) prior to tissue diagnosis. The maxSUV(maximum value of SUV) were calculated and compared between benign and malignant lesions. The lesion analysis was based on the transverse whole body image. The maxSUV with cutoff of 4.1 was used in distinguishing benign from malignant soft tissue tumor and 3.05 was used in bone tumor by ROC curve. Results: There was a statistically significant difference in maxSUV between benign (n=11; maxSUV $3.4{\pm}3.2$) and malignant (n=12; maxSUV $14.8{\pm}12.2$) lesions in soft tissue tumor (p=0.001). Between benign bone tumor (n=9; maxSUV $5.4{\pm}4.0$) and malignant bone tumor (n=14; maxSUV $7.3{\pm}3.2$), there was not a significant difference in maxSUV. The sensitivity and specificity for differentiating malignant from benign soft tissue tumor was 83% and 91%, respectively. There were four false positive malignant bone tumor cases to include fibrous dysplasia, Langerhans-cell histiocytosis (n=2) and osteoid osteoma. Also, one false positive case of malignant soft tissue tumor was nodular fasciitis. Conclusion: The maxSUV was useful for differentiation of benign from malignant lesion in primary soft tissue tumors. In bone tumor, the low maxSUV correlated well with benign lesions but high maxSUV did not always mean malignancy.

Development of an Official Analytical Method for Determination of Phorate and its Metabolites in Livestock Using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 Phorate 및 대사산물 5종 동시분석법 개발)

  • Ko, Ah-Young;Kim, Heejung;Jang, Jin;Lee, Eun Hyang;Ju, Yunji;Noh, Mijung;Kim, Seongcheol;Park, Sung-Won;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.30 no.3
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    • pp.272-280
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    • 2015
  • A simultaneous official method was developed for the determination of phorate and its metabolites (phorate sulfoxide, phorate sulfone, phorate oxon, phorate oxon sulfoxide, phorate oxon sulfone) in livestock samples. The analytes were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Phorate and its metabolites were extracted from beef and milk samples with acidified acetonitrile (containing 1% acetic acid) and partitioned with anhydrous magnesium sulfate. Then, the extract was purified through primary secondary amine (PSA) and C18 dispersive sorbent. Matrix matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/L) for all the analytes into blank extract with $r^2$ > 0.996. For validation purposes, recovery studies were carried out at three different concentration levels (beef 0.004, 0.04 and 0.2 mg/kg; milk 0.008, 0.04 and 0.2 mg/kg, n = 5). The recoveries were within 79.2-113.9% with relative standard deviations (RSDs) less than 19.2% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines. The limit of quantification was quite lower than the maximum residue limit (MRL) set by the Ministry of Food and Drug Safety (0.05 mg/kg). The proposed analytical method was accurate, effective and sensitive for phorate and its metabolites determination and it will be used to as an official analytical method in Korea.

Levels of Plasma Glucose and Lipid in Rats Fed Bread Supplemented with Natural Extracts (천연추출물이 첨가된 식빵을 섭취한 흰쥐의 혈당 및 지질수준에 미치는 영향)

  • Kim, Se-Wook;Han, Ah-Ram;Chun, Su-Hyun;Nam, Mi-Hyun;Hong, Chung-Oui;Kim, Bok Hee;Kim, Tae Cheol;Lee, Kwang-Won
    • Korean Journal of Food Science and Technology
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    • v.48 no.1
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    • pp.77-85
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    • 2016
  • In this study, 4-week-old rats were fed bread supplemented with Terminalia chebula (TC), Plantago asiatica (PA), Linder obtusiloba (LO), and Capsosiphon fulvescens (CF) ethanol extracts, to determine the decrease in blood glucose levels, as well as the anti-inflammatory and lipid-enhancing effects. Previous studies have demonstrated the antioxidative effects of these ethanol extracts. After sacrifice, the liver tissue, whole blood, and serum samples were collected for biochemical analysis. The results showed a significant decrease in blood glucose level, lipid peroxidation, malondialdehyde (MDA) level, HbA1c level, total cholesterol, and low-density lipoprotein (LDL)-cholesterol (p<0.05) and an increase in high-density lipoprotein (HDL)-cholesterol level in rats fed bread supplemented with LO and CF ethanol extracts (p<0.05). Therefore, the results of this study demonstrate that bread supplemented with LO and CF ethanol extracts can potentially affect the blood glucose level and lead to lipid enhancement.