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Determination of Dithiocarbamates in Agricultural Products Circulated in Korea (시판 농산물의 dithiocarbamates 분석)

  • Kim, Hee-Yun;Choi, Hee-Ju;Eom, Ji-Yoon;Seo, Eun-Chae;Choi, Sung-Hee;Cheong, So-Young;Choi, Sun-Hee;Lee, Hwa-Jeong;Choi, Jae-Chun
    • Korean Journal of Food Science and Technology
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    • v.42 no.1
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    • pp.1-7
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    • 2010
  • To revise the dithiocarbamates residue analysis method and survey the residues in agricultural products that were treated with these fungicides in Korea, we purchased 20 types of foodstuffs (rice, potato, cabbage, apple etc.) from markets in five major cities. 236 samples of the purchased foodstuffs were then analyzed for the presence of dithiocarbamates by HPLC/UV and HPLC/APCI-MS. The $R^2$, LOD and LOQ in the range of 0.5-107.3 mg/L were as follows: DCC: y=174.34x+18.315, $R^2=0.9999$, 0.01 mg/L, and 0.04 mg/L; EBDC: y=227.38x-14.715, $R^2=1.0000$, 0.01 mg/L and 0.02 mg/L; PBDC: y=38.46x-21.412, $R^2=0.9999$, 0.04 mg/L, and 0.1 mg/L; ETU: y=52.752x-4.4819, $R^2=0.9998$, 0.02 mg/L and 0.03 mg/L; PTU: y=128.28x+4.4624, $R^2=0.9998$, 0.02 mg/L, and 0.04 mg/L. The levels of DDC, EBDC, PBDC, ETU and PTU in 20 agricultural products fortified to 10.0-107.3 mg/L ranged from 61.7-117.5%, 65.3-110.1%, 61.5-109.6%, 69.3-116.3% and 70.2-97.2%, respectively. Overall, dithiocarbamates were detected in 100 samples and the detection ratio was 42.4%. Among these, only 3 samples (1.3%) of Lycii fructus had residue levels that were above the action limits, while the remaining samples (233 samples) contained levels of dithiocarbamates below the detection limit or below the Korea MRLs (Maximum Residue Limits).

Monitoring of Pesticides in the Yeongsan and Seomjin River Basin (영산강 및 섬진강 수계 중 농약 분포 조사)

  • Lee, Young-Jun;Choi, Jeong-Heui;Kim, Sang Don;Jung, Hee-Jung;Lee, Hyung-Jin;Shim, Jae-Han
    • Korean Journal of Environmental Agriculture
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    • v.34 no.4
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    • pp.274-281
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    • 2015
  • BACKGROUND: A lasting release of low levels of persistence chemicals including pesticides and pharmaceuticals into river has a bad influence on aquatic ecosystems and humans. The present study monitored pesticide residues in the Yeongsan and Seomjin river basins and their tributaries as a fundamental study for water quality standard of pesticides.METHODS AND RESULTS: Nine pesticides(aldicarb, carbaryl, carbofuran, chlorpyrifos, 2,4-D, MCPA, methomyl, metolachlor, and molinate) were determined from water samples using SPE-Oasis HLB(pH 2) and LC/MS/MS. Validation of the method was conducted through matrix-matched internal calibration curve, method detection limit(MDL), limit of quantification(LOQ), accuracy, precision, and recovery. MDLs of all pesticides satisfied the GV/10 values. Linearity(r2) was 0.9965- 0.9999, and a percentage of accuracy, precision, and recovery was 89.4-113.6%, 3.1-14.0%, and 90.8-106.2%, respectively. All pesticides exclusive of aldicarb were determined in the river samples, and there was a connection between the positive monitoring results and agricultural use of the pesticides.CONCLUSION: Monitoring outcomes of the present study implied that pesticides were a possible non-point pollutant source in the Yeongsan and Seomjin river basins and tributaries. Therefore, it is required to produce and accumulate more monitoring results on pesticides in river waters to set water quality standards, finally to preserve aquatic ecosystems.

Risk Assessment Aluminum Levels of Circulating Agricultural Products in Korea (국내 다소비 농산물의 알루미늄 농도 모니터링 및 농산물 섭취로 인한 위해도 평가)

  • An, Jae-Min;Hong, Kyong-Suk;Kim, Sung-Youn;Kim, Ji-Hye;Yu, Kyong-Eun;Kim, Hyo-Young;Park, Hyoung-Dal;Lee, Jae-Hwon;Kim, Dong-Ho
    • Korean Journal of Environmental Agriculture
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    • v.34 no.4
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    • pp.336-344
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    • 2015
  • BACKGROUND: This study was carried out to collect occurrence data on aluminum in 12 type agricultural products and assess dietary exposure risk to the Korean population health for aluminum concentration in agricultural products.METHODS AND RESULTS: Aluminum analysis samples were performed using microwave device and Inductively Coupled Plasma Optical Emission Spectrometer. The LOD(Limit of Detection) for aluminum was 0.851 μg/kg, while the LOQ(Limit of Quantitation) was 2.838 μg/kg and recovery was 97.6% for aluminum. The average levels of aluminum in mg/kg were 0.526 for rice, 0.546 for Korean cabbage, 1.316 for corn, 6.207 for soybean, 0.549 for sweet potato, 0.257 for potato, 6.963 for spinach, 1.213 for carrot, 0.524 for garlic, 0.950 for radish, 1.015 for leek, and 3.511 for Welsh onion. The dietary exposures of aluminum through usual intake were polished rice 89.31 μg/day, Korean cabbage 33.14 μg/day, corn 0.66 μg/day, soybean 3.72 μg/day, sweet potato 6.86 μg/day, potato 4.96 μg/day, spinach 45.96 μg/day, carrot 6.79 μg/day, garlic 2.36 μ g/day, radish 7.32 μg/day, leek 2.23 μg/day and Welsh onion 43.89 μg/day, taking 0.57%, 0.21%, 0.00%, 0.02%, 0.04%, 0.03%, 0.04%, 0.04%, 0.02%, 0.05%, 0.01% and 0.28% of PTWI(2 mg/kg b.w./week), respectively.CONCLUSION: The levels of overall dietary exposure to aluminum for Korean population through intake of agricultural product was far below the recommended JECFA level, indicating of least possibility of risk.

Determination of Carazolol and Azaperone in Livestock and Fishery Products Using Liquid Chromatography-tandem Mass Spectrometry (축수산물에서 LC-MS/MS를 이용한 카라졸롤 및 아자페론 분석)

  • Choi, Soo Yeon;Kang, Hui-Seung;Kim, Joohye;Cheon, So-Young;Jeong, Jiyoon;Cho, Byung-Hoon;Lee, Kang-Bong
    • Journal of Food Hygiene and Safety
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    • v.33 no.3
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    • pp.176-184
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    • 2018
  • The aim of the present work was to develop simultaneous methods of quantification of carazolol, azaperone, and azaperol residues in livestock and fishery products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Samples were extracted from beef, pork, chicken, egg, milk and shrimp using acetonitrile (ACN); while flat fish and eel were extracted using 80% ACN. For purification, ACN saturated n-hexane was used to remove fat composition. The standard calibration curves showed good linearity as correlation coefficients; $r^2$ was > 0.99. Average recoveries expressed were within the range of 67.9-105% for samples fortified at three different levels ($0.5{\times}MRL$, $1{\times}MRL$ and $2{\times}MRL$). The correlation coefficient expressed as precision was within the range of 0.55-7.93%. The limit of quantification (LOQ) was 0.0002-0.002 mg/kg. The proposed analytical method showed high accuracy and acceptable sensitivity based on Codex guideline requirements (CAC/GL71-2009). This method can be used to analyze the residue of carazolol, azaperone, and azaperol in livestock and fishery products.

Monitoring of Heavy Metals Migrated from Glassware, Ceramics, Enamelware, and Earthenware (유리제, 도자기제, 법랑 및 옹기류 재질의 식품용 기구 및 용기·포장의 중금속 이행량 모니터링)

  • Cho, Kyung Chul;Jo, Ye-Eun;Park, So-Yeon;Park, Yongchjun;Park, Se-Jong;Lee, Hye Young
    • Journal of Food Hygiene and Safety
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    • v.35 no.1
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    • pp.23-30
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    • 2020
  • This study investigated the migration levels of lead (Pb), cadmium (Cd), and arsenic (As) from food contact articles (glassware, ceramics, enamelware, and earthenware) into a food stimulant (4% v/v, acetic acid). Migration tests were performed at 25℃ for 24 h and all analyses were performed using Inductively-Coupled Plasma Mass Spectrometry (ICP-MS). The method was validated by linearity of calibration curves, limit of detection (LOD), limit of quantification (LOQ), recovery, precision, and uncertainty. In glassware, the migration concentrations ranged from not-detected (N.D.) to 752.21 ㎍/L and N.D. to 1.99 ㎍/L for Pb and Cd, respectively. In ceramics, the migration concentrations ranged from N.D. to 1,955.86 ㎍/L, N.D. to 74.06 ㎍/L, and N.D. to 302.40 ㎍/L for Pb, Cd, and As, respectively. In enamelware, the migration concentrations ranged from N.D. to 4.48 ㎍/L, N.D. to 7.00 ㎍/L, and N.D. to 52.00 ㎍/L for Pb, Cd, and Sb, respectively. In earthenware, the migration concentrations ranged from N.D. to 13.68 ㎍/L, N.D. to 0.04 ㎍/L, and N.D. to 6.71 ㎍/L for Pb, Cd, and As, respectively. All results were below the migration limits of Korea standards and specifications for food utensils, containers, and packages.

Monitoring and Risk Assessment of Pesticide Residues on Stalk and Stem Vegetables Marketed in Incheon Metropolitan Area (인천광역시 유통 엽경채류 농산물의 잔류농약 실태조사 및 위해성 평가)

  • Park, Byung-Kyu;Jung, Seung-Hye;Kwon, Sung-Hee;Ye, Eun-Young;Lee, Han-Jung;Seo, Soon-Jae;Joo, Kwang-Sig;Heo, Myung-Je
    • Journal of Food Hygiene and Safety
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    • v.35 no.4
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    • pp.365-374
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    • 2020
  • This study was conducted to monitor the residual pesticides on a total of 320 stalk and stem vegetables from January 2019 to December 2019 in the Incheon metropolitan area. Pesticide residues in samples were analyzed by the multi-residue method for 373 pesticides using GC-MS/MS, LC-MS/MS, GC-ECD, GC-NPD and HPLC-UVD. Risk assessment was also carried out based on the amount of stalk and stem vegetables consumed. The linearity correlation coefficient for the calibration curve was 0.9951 to 1.0000, LOD 0.002 to 0.022 mg/kg, LOQ 0.005 to 0.066 mg/kg and recovery was 82.0 to 108.0%. According to the monitoring of pesticides, 36 (11.3%) of 320 were detected with pesticide residues and 3 (0.9%) samples exceeded the maximum residual limit. The detection frequency for Chinese chives and Welsh onion was higher than that for other stalk and stem vegetables. The frequently detected pesticides were etofenprox, procymidone, fludioxonil, and pendimethalin. As a tool of risk assessment through the consumption of pesticide detectable agricultural products, the ratio of estimated daily intake (EDI) to acceptable daily intake (ADI) was calculated in the range of 0.0062-24.1423%. These results indicate that there is no particular health risk through consumption of commercial stalk and stem vegetables detected with pesticide residues.

Isolation, Quality Evaluation, and Seasonal Changes of Bakkenolide B in Petasites japonicus by HPLC (머위로부터 Bakkenolide B의 순수분리, HPLC분석 방법 및 채취 시기별 함량 분석)

  • Kim, Tae Hoon;Kim, Do Youn;Jung, Won Jung;Nagaiya, Ravichandran;Son, Beung Gu;Park, Young Hoon;Kang, Jum Soon;Lee, Young Jae;Im, Dong-Soon;Lee, Young-Geun;Choi, Yung Hyun;Choi, Young-Whan
    • Journal of Life Science
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    • v.24 no.3
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    • pp.252-259
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    • 2014
  • The leaves of Peatasites japonicus are a traditional oriental medicine with diverse biological activities. A simple and specific analytical method for the quantitative determination of bakkenolide B constituents from methanolic extract of the leaves of P. japonicus was developed. Bakkenolide B was isolated from the leaves of P. japonicus, and its structure was elucidated based on 1D, 2D NMR, and GC-MS spectral data. A liquid chromatographic method was developed to evaluate the quality of P. japonicus through determination of major active compound, bakkenolide B. The wavelengths at 254 and 215 nm were chosen to determine bakkenolide B. The recovery of the method was in the range of 98.6 to 103.1%, and bakkenolide B showed good linearity ($r^2$=0.999) within test ranges. The developed method was applied to the determination of bakkenolide B in the plant part and seasonal changes. The results showed that the content of bakkenolide B in the leaf was higher than in the petiole and rhizome. In this study, a simple, rapid, and reliable high-performance liquid chromatography method was used to determine the percentage and composition of bakkenolide B in P. japonicus procured from different Petasites species plants in South Korea. The method can be employed in routine quantitative analysis and quality control of different products in the market.

Method Validation and Quantification of Lutein and Zeaxanthin from Green Leafy Vegetables using the UPLC System (UPLC를 이용한 lutein과 zeaxanthin의 분석법 검증 및 엽채류에서의 정량적 평가)

  • Kim, Suna;Kim, Ji-Sun
    • Korean Journal of Food Science and Technology
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    • v.44 no.6
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    • pp.686-691
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    • 2012
  • The objective of this research is to present method development and validation for the simultaneous determination of lutein and zeaxanthin using ultra performance liquid chromatography (UPLC). Also, rapid quantification was performed on six green leafy vegetables (Allium tuberosum, Aster scaber, Hemerocallis fulva, Pimpinella brachycarpa, Sedum sarmentosum and Spinacia oleracea) that are commonly consumed in Korea. Separation and quantification were successfully achieved with a Waters Acquity BEH C18 ($50{\times}2.1mm$, $1.7{\mu}m$) column by 85% methanol within 5 min. Two compounds showed good linearity ($r^2$ > 0.9968) in $1-150{\mu}g/mL$. Limit of detection (LOD) and quantification (LOQ) for lutein and zeaxanthin were 1.7 and 5.1 g/mL and 2.1 and 6.3 g/mL, respectively. The RSD for intra- and inter-day precision of each compound was less than 10.69%. The recovery of each compound was in the range of 91.75-105.13%. Aster scaber and Spinacia oleracea contained significantly higher amounts of lutein ($4.06{\pm}0.24$ and $3.97{\pm}0.10mg$/100 g of fresh weight), respectively.

A Study on Heavy Metal Contents in Processed Foods and Their Safety Evaluations (가공식품 중 중금속 함량 및 안전성 평가)

  • Lee, Hyo-Jung;Shim, Jee-Youn;Oh, Hyun-Suk;Jang, Mi-Ran;Lee, Yoon-Ae;Lee, Ryun-Kyung;Kim, Min-A;Lee, Sang-Min;Cho, Tae-Yong;Kang, Ho-Il
    • Korean Journal of Food Science and Technology
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    • v.44 no.1
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    • pp.21-27
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    • 2012
  • This research was carried out as a survey on the contents of lead, cadmium, and arsenic in processed foods (milk, vegetable oil, and margarine) in Korea. The limits of quantification (LOQs) were Pb 0.3 ${\mu}g/kg$, Cd 0.15 ${\mu}g/kg$, and As 0.45 ${\mu}g/kg$ for milk and Pb 0.61 ${\mu}g/kg$, Cd 0.31 ${\mu}g/kg$, and As 0.91 ${\mu}g/kg$ for vegetable oil and margarine. The recoveries were 92.6-98.0% for Pb, 91.2-98.9% for Cd, and 97.9-104.7% for As. The average levels of Pb were 2.395 ${\mu}g/kg$ for milk, and 7.656 ${\mu}g/kg$ for vegetable oil. The average levels of Cd were 0.483 ${\mu}g/kg$ for milk, and 0.380 ${\mu}g/kg$ for vegetable oil, and levels of As were 0.781 ${\mu}g/kg$ for milk, and 1.241 ${\mu}g/kg$ for vegetable oil. The results of this study showed that Pb, Cd, and As contents in the whole samples were less than the maximum residual levels in the processed foods that were specified by the Codex standard.

Method Validation for the Determination of Eleutherosides and β-Glucan in Acanthopanax koreanum (탐라오가피의 Eleutheroside B, E 및 β-Glucan 함량 분석 및 분석법 검증)

  • Kim, Young-Hyun;Bae, Da-Bin;Park, Sun-Ok;Lee, Sang-Jong;Cho, Ok-Hyun;Lee, Ok-Hwan
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.42 no.9
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    • pp.1419-1425
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    • 2013
  • The aim of this study was to investigate the method validation for the determination of eleutherosides (B and E) and ${\beta}$-glucan in Acanthopanax (A.) koreanum. This medicinal plant reportedly mainly included eleutherosides which exhibit the pharmacological effects, and ${\beta}$-glucan substantially enhances the function of the immune system by activating macrophages. The specificity, linearity, precision, accuracy, limit of detection (LOD, S/N=3), and limit of quantification (LOQ, S/N=10) were measured by HPLC and enzymatic methods. Our results showed that the coefficient of calibration correlation ($R^2$) for eleutheroside B and E were 0.9997 and 0.9999, respectively. The limits of detection (LOD) for eleutheroside B and E were $0.050{\mu}g/mL$ and $0.025{\mu}g/mL$, respectively. The recovery rate of eleutheroside B and E were revealed in the high range of 100.66~110.04% and 94.26~111.62%, respectively. The inter-day precision of eleutheroside B and E in the root and stem in A. koreanum were 1.4~5.0% and 1.1~2.5%, respectively. The intra-day precision of eleutheroside B and E in the root and stem in A. koreanum were 2.8~2.9% and 0.4~1.1%, respectively. Furthermore, the inter-day and intra-day precision of ${\beta}$-glucan in the stem, leaf, and fruit of A. koreanum were 1.32~5.67% and 8.01~11.76%, respectively. In conclusion, the methods were validated for the detection of eleutherosides and ${\beta}$-glucan in A. koreanum.