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Development and Validation of an Analytical Method for Fungicide Fluoxastrobin Determination in Agricultural Products (농산물 중 살균제 Fluoxastrobin의 시험법 개발 및 유효성 검증)

  • So Eun, Lee;Su Jung, Lee;Sun Young, Gu;Chae Young, Park;Hye-Sun, Shin;Sung Eun, Kang;Jung Mi, Lee;Yun Mi, Chung;Gui Hyun, Jang;Guiim, Moon
    • Journal of Food Hygiene and Safety
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    • v.37 no.6
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    • pp.373-384
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    • 2022
  • Fluoxastrobin a fungicide developed from Strobilurus species mushroom extracts, can be used as an effective pesticide to control fungal diseases. In this study, we optimized the extraction and purification of fluoxastrobin according to its physical and chemical properties using the QuEChERS method and developed an LC-MS/MS-based analysis method. For extraction, we used acetonitrile as the extraction solvent, along with MgSO4 and PSA. The limit of quantitation of fluoxastrobin was 0.01 mg/kg. We used 0.01, 0.1, and 0.5 mg/kg of five representative agricultural products and treated them with fluoxastrobin. The coefficients of determination (R2) of fluoxastrobin and fluoxastrobin Z isomer were > 0.998. The average recovery rates of fluoxastrobin (n=5) and fluoxastrobin Z isomer were 75.5-100.3% and 75.0-103.9%, respectively. The relative standard deviations (RSDs) were < 5.5% and < 4.3% for fluoxastrobin and fluoxastrobin Z isomer, respectively. We also performed an interlaboratory validation at Gwangju Regional Food and Drug Administration and compared the recovery rates and RSDs obtained for fluoxastrobin and fluoxastrobin Z isomer at the external lab with our results to validate our analysis method. In the external lab, the average recovery rates and RSDs of fluoxastrobin and fluoxastrobin Z isomer at each concentration were 79.5-100.5% and 78.8-104.7% and < 18.1% and < 10.2%, respectively. In all treatment groups, the concentrations were less than those described by the 'Codex Alimentarius Commission' and the 'Standard procedure for preparing test methods for food, etc.'. Therefore, fluoxastrobin is safe for use as a pesticide.

Development of Analytical Method for Detection of Fungicide Validamycin A Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Validamycin A의 시험법 개발)

  • Park, Ji-Su;Do, Jung-Ah;Lee, Han Sol;Park, Shin-min;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.1
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    • pp.22-29
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    • 2019
  • Validamycin A is an aminoglycoside fungicide produced by Streptomyces hygroscopicus that inhibits trehalase. The purpose of this study was to develop a method for detecting validamycin A in agricultural samples to establish MRL values for use in Korea. The validamycin A residues in samples were extracted using methanol/water (50/50, v/v) and purified with a hydrophilic-lipophilic balance (HLB) cartridges. The analyte was quantified and confirmed by 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 (0.005~0.5 ng) into a blank extract with $R^2$ > 0.99. The limits of detection and quantification were 0.005 and 0.01 mg/kg, respectively. For validation validamycin A, recovery studies were carried out three different concentration levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) with five replicates at each level. The average recovery range was from 72.5~118.3%, with relative standard deviation (RSD) less than 10.3%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the NIFDS (National Institute of Food and Drug Safety) guideline (2016). Therefore, the proposed analytical method is accurate, effective and sensitive for validamycin A determination in agricultural commodities.

Roles of ginsenosides in sepsis

  • Tao Yu;Yidi Tang;Fenglan Zhang;Leiming Zhang
    • Journal of Ginseng Research
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    • v.47 no.1
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    • pp.1-8
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    • 2023
  • The herbal medication Panax ginseng Meyer has widespread use in China, Korea, and other parts of the world. The main constituents of ginseng are ginsenosides, which include over 30 different triterpene saponins. It has been found that ginsenosides and their metabolites including Rg1, compound K, Rb1, Re, Rg3, and Rg5 exert anti-inflammatory activities by binding to the glucocorticoid receptor, modulating inflammation-related signaling, including NF-κB and MAPK signaling, and reducing levels of proinflammatory cytokines. Here, we review the recent literature on the molecular actions of ginsenosides in sepsis, suggesting ways in which they may be used to prevent and treat the disease.

Development of analytical method for cyantraniliprole residues in welsh onion (Allium species) (대파(Allium속)에서 살충제 Cyantraniliprole 잔류분석을 위한 시험법 개발)

  • Do, Jung-Ah;Lee, Mi-Young;Chang, Moon-Ik;Hong, Jin-Hwan;Oh, Jae-Ho
    • Analytical Science and Technology
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    • v.28 no.3
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    • pp.175-181
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    • 2015
  • Cyantraniliprole, which is an ananthranilic diamide insecticide that was developed by the DuPont Corporation, was registered in the Republic of Korea in 2012. It offers exceptional insecticidal activity on a broad range of Lepidopera, Coleoptera, Diptera, and Isoptera. The maximum residue limits are set to pepper, peach, apple, sweet pepper, welsh onion, and so on (0.2~2.0 mg/kg). Therefore, an analytical method for determining cyantraniliprole residue in agricultural products was developed to ensure food safety. In previous studies, welsh onions were among vegetables included in the allium species, which is a representative plant with sulfur organic compounds. In this study, the analytical method was developed and evaluated for the elimination of sulfur compounds from the test solution of allium species during pesticide residue analysis. In order to inactivate the enzyme allinase and produce sulfur compounds, sample extraction was made in the base state pH 10 by reducing the activity of the enzyme. The recoveries of the developed method ranged from 81.9% to 83.2%, and the relative standard deviations were less than 10%. Therefore, based on the results, the method developed in this study is accurate and appropriate for use in cyantraniliprole determination. It will be used as the official method for managing the safety of cyantraniliprole residues in agricultural products.

The Establishing Test Method of Bactericidal Activity and the Evaluating of Korean Disinfectants/Sanitizers Efficacy (살균소독력 시험법 확립 및 살균소독력 평가)

  • Kim, Hyung-Il;Lee, Kwang-Ho;Kwak, In-Shin;Eom, Mi-Ok;Jeon, Dae-Hoon;Sung, Jun-Hyun;Choi, Jung-Mi;Kang, Han-Saem;Kim, Yong-Soo;Kang, Kil-Jin
    • Korean Journal of Food Science and Technology
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    • v.37 no.5
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    • pp.838-843
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    • 2005
  • Bacterial suspension test was used to establish Standardization Test Method to investigate bactericidal activity of disinfectant/sanitizer product. Using acceptable verification methodology, test substance showing 5 log or higher reduction in viable count against Escherichia coli ATCC 10536 and Staphylococcus aureus ATCC 6538, representing Gram-negative and -positive bacteria, respectively, under test conditions for $5\;min{\pm}10\;sec\;at\;20{\pm}1^{\circ}C$ was considered to have sanitizing capability. All disinfectant/sanitizer products tested under manufacturer's recommended in-use condition gave good reduction values against major food-poisoning bacteria. This standardized method was valuable for evaluating efficacy of disinfectants/sanitizers and could be used as Standardization Test Method for assessing bactericidal activity

Development and Utilization of KASP Markers for the Identification of Three Types of Ephedra Herbs (마황 3종 판별을 위한 KASP 마커 개발과 활용)

  • Boreum, Park;Sun Hee, Lee;Kyung-Moon, Han;Jin Woo, Hwang;Hyung il, Kim;Sun Young, Baek
    • Korean Journal of Pharmacognosy
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    • v.53 no.4
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    • pp.226-233
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    • 2022
  • Ephedra herbs are defined as stem of Ephedra sinica , Ephedra intermedia and Ephedra equisetina in the Korean Pharmacopoeia. It is important to use pure herbs to derive the safety and efficacy of herbal medicine. However, the identification of these herbs by conventional taxonomic methods is difficult. Recently, many studies have applied these DNA barcoding for the identification of herbal medicinal species using standard DNA markers. In this study, we report a case study in which the identification of Ephedra species was done by DNA barcoding. For identification of Ephedra species, 17 samples were collected, and a reference DNA barcode library was developed using 6 markers (rbcL, matK, ITS2, ycf1, ycf3, and rpoC2). To develop KASP-SNP markers, we selected 4 markers (ycf1, ycf3, rpl2, and rbcL), which were able to distinguish three Ephedra species. In the result, the specific markers for each of the three Ephedra were clustered into FAM-positive section, whereas non-targeted plants were clustered either HEX-positive or negative section. Therefore, we have developed KASP assay that allow rapid and easy Ephedra species identification using three KASP markers.

Establishment of an Analytical Method for Prometryn Residues in Clam Using GC-MS (GC-MS를 이용한 바지락 중 prometryn 잔류분석법 확립)

  • Chae, Young-Sik;Cho, Yoon-Jae;Jang, Kyung-Joo;Kim, Jae-Young;Lee, Sang-Mok;Chang, Moon-Ik
    • Korean Journal of Food Science and Technology
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    • v.45 no.5
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    • pp.531-536
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    • 2013
  • We developed a simple, sensitive, and specific analytical method for prometryn using gas chromatography-mass spectrometry (GC-MS). Prometryn is a selective herbicide used for the control of annual grasses and broadleaf weeds in cotton and celery crops. On the basis of high specificity, sensitivity, and reproducibility, combined with simple analytical operation, we propose that our newly developed method is suitable for use as a Ministry of Food and Drug Safety (MFDS, Korea) official method in the routine analysis of individual pesticide residues. Further, the method is applicable in clams. The separation condition for GC-MS was optimized by using a DB-5MS capillary column ($30m{\times}0.25mm$, 0.25 ${\mu}m$) with helium as the carrier gas, at a flow rate of 0.9 mL/min. We achieved high linearity over the concentration range 0.02-0.5 mg/L (correlation coefficient, $r^2$ >0.998). Our method is specific and sensitive, and has a quantitation limit of 0.04 mg/kg. The average recovery in clams ranged from 84.0% to 98.0%. The reproducibility of measurements expressed as the coefficient of variation (CV%) ranged from 3.0% to 7.1%. Our analytical procedure showed high accuracy and acceptable sensitivity regarding the analytical requirements for prometryn in fishery products. Finally, we successfully applied our method to the determination of residue levels in fishery products, and showed that none of the analyzed samples contained detectable amounts of residues.

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.

In Vitro Evaluation of Three Positional Isomers of mono-PEGylated Salmon Calcitonin

  • Jung, J.Y.;Youn, Y.S.;Oh, S.H.;Hong, S.T.;Lee, J.E.;Lee, S.O.;Lee, K.C.
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.300.1-300.1
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    • 2003
  • Salmon calcitonin (sCT) is a therapeutic polypeptide hormone consisting of 32 amino acids (3432 Da). As with other bioactive peptide therapeutics, however, therapeutic use of sCT has been limited due to the problems of short circulating half-life and rapid proteolytic degradation. To get over this problem, the three positional isomers of mono-PEGylated sCT were prepared and among these, the best drug candiate for nasal application was chosen. (omitted)

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Acute and repeated dose 26-week oral toxicity study of 20(S)-ginsenoside Rg3 in Kunming mice and Sprague-Dawley rats

  • Li, Chunmei;Wang, Zhezhe;Li, Guisheng;Wang, Zhenhua;Yang, Jianrong;Li, Yanshen;Wang, Hongtao;Jin, Haizhu;Qiao, Junhua;Wang, Hongbo;Tian, Jingwei;Lee, Albert W.;Gao, Yonglin
    • Journal of Ginseng Research
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    • v.44 no.2
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    • pp.222-228
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    • 2020
  • Background: 20(S)-ginsenoside-Rg3 (C42H72O13), a natural triterpenoid saponin, is extracted from red ginseng. The increasing use of 20(S)-ginsenoside Rg3 has raised product safety concerns. Methods: In acute toxicity, 20(S)-ginsenoside Rg3 was singly and orally administrated to Kunming mice and Sprague-Dawley (SD) rats at the maximum doses of 1600 mg/kg and 800 mg/kg, respectively. In the 26-week toxicity study, we used repeated oral administration of 20(S)-ginsenoside Rg3 in SD rats over 26 weeks at doses of 0, 20, 60, or 180 mg/kg. Moreover, a 4-week recovery period was scheduled to observe the persistence, delayed occurrence, and reversibility of toxic effects. Results: The result of acute toxicity shows that oral administration of 20(S)-ginsenoside Rg3 to mice and rats did not induce mortality or toxicity up to 1600 and 800 mg/kg, respectively. During a 26-week administration period and a 4-week withdrawal period (recovery period), there were no significant differences in clinical signs, body weight, food consumption, urinalysis parameters, biochemical and hematological values, or histopathological findings. Conclusion: The mean oral lethal dose (LD50) of 20(S)-ginsenoside Rg3, in acute toxicity, is above 1600 mg/kg and 800 mg/kg in mice and rats, respectively. In a repeated-dose 26-week oral toxicity study, the no-observed-adverse-effect level for female and male SD rats was 180 mg/kg.