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Development and validation of an analytical method for fungicide fenpyrazamine determination in agricultural products by HPLC-UVD (HPLC-UVD를 이용한 살균제 fenpyrazamine의 시험법 개발 및 검증)

  • Park, Hyejin;Do, Jung-Ah;Kwon, Ji-Eun;Lee, Ji-Young;Cho, Yoon-Jae;Kim, Heejung;Oh, Jae-Ho;Rhee, Kyu-Sik;Lee, Sang-Jae;Chang, Moon-Ik
    • Analytical Science and Technology
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    • v.27 no.3
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    • pp.172-180
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    • 2014
  • Fenpyrazamine which is a pyrazole fungicide class for controlling gray mold, sclerotinia rot, and Monilinia in grapevines, stone fruit trees, and vegetables has been registered in republic of Korea in 2013 and the maximum residue limits of fenpyrazamine is set to grape, peach, and mandarin as 5.0, 2.0, and 2.0 mg/kg, respectively. Very reliable and sensitive analytical method for determination of fenpyrazamine residues is required for ensuring the food safety in agricultural products. Fenpyrazamine residues in samples were extracted with acetonitrile, partitioned with dichloromethane, and then purified with silica-SPE cartridge and eluted with hexane and acetone mixture. The purified samples were determined by HPLC-UVD and confirmed with LC-MS and quantified using external standard method. Linear range of fenpyrazamine was between $0.1{\sim}5.0{\mu}g/mL$ with the correlation coefficient (r) 0.999. The average recovery ranged from 71.8 to 102.7% at the spiked level of 0.05, 0.5, and 5.0 mg/kg, while the relative standard deviation was between 0.1 and 7.3%. In addition, limit of detection and limit of quantitation were 0.01 and 0.05 mg/L, respectively. The results revealed that the developed and validated analytical method is possible for fenpyrazamine determination in agricultural product samples and will be used as an official analytical method.

Studies on Processing ana Keeping Quality of Retort Pouched Foods (3) Preparation and Keeping Quality of Retort Pouched Fried Mackerel Meat Paste (레토르트파우치식품의 가공 및 품질안정성에 관한 연구 (3) 레토르트파우치 튀김어묵의 제조 및 저장중의 품질안정성)

  • LEE Eung-Ho;OH Kwang-Soo;KOO Jae-Geun;PARK Hyang-Suk;CHO Soon-Yeong;CHA Yong-Jun
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.17 no.5
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    • pp.373-382
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    • 1984
  • Processing conditions of retort pouched fried mackerel fish meat paste and quality stability during storage were investigated. The reasonable amounts of added ingredients to the frozen mackerel meat paste were $10\%$ of corn starch, $1\%$ of soybean protein, $1.5\%$ of sodium chloride, $0.6\%$ of monosodium glutamate, $0.3\%$ of alcoholic extract of red pepper, and $0.1\%$ of sodium erythorbate as an antioxidant and also added water corresponding to $10\%$ of the frozen mackerel meat paste. After grinding the defrosted mackerel fish meat paste with ingredients, the meat paste was molded in bar type and fried in soybean oil at $170-180^{\circ}C$ for 3 minutes. The fried mackerel meat paste was cooled, vacuum-packed in laminated plastic film bag (polyester/polyvinylidene chloride/unoriented polypropylene : $12{\mu}m/15{\mu}/50{\mu}m,\;14{\times}19cm$) and finally sterilized at $120^{\circ}C$ for 20 minutes in a hot water circulating retort. The pH, volatile basic nitrogen, moisture content, water activity, color, thiobarbituric acid value, peroxide value, texture and viable bacterial count of products were examined during 100 days of storage at $25{\pm}3^{\circ}C\;and\;5^{\circ}C$. The results showed that products could be preserved in good condition for 100 days at $25{\pm}3^{\circ}C$. Judging from sensory evaluation, the quality of products was not inferior to that of market products.

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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.

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.

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.

Effects of the Supplementation of Fermented Food Wastes on the Performances of Pigs (발효 남은 음식물의 급여가 비육돈의 생산성에 미치는 영향)

  • Jo Ik-Hwan;Kim Guk-Won;Lee Sung-Hun
    • Korean Journal of Organic Agriculture
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    • v.13 no.3
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    • pp.315-332
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    • 2005
  • This study was conducted to assess the nutritional value and the safety of the fermented food wastes (FFW) made by adding lactobacillus spp. and bacillus spp. at the ratio of 3:7, respectively to food wastes collected everywhere, and also to determine effects on the performances, carcass characteristics and economical profitability when FFW was fed to pigs. For swine trial, FFW was formulate to pellet by utilizing different feed ingredients, and its formulated FFW pellet was used in this feeding trial. Treatments were consisted of different ratios (T1: $100+0\%$, T2: $75+25\%$, T3: $50+50\%$, T4: $25+75\%$, T5: $0+100\%$) of FFW pellet to commercial diet. A total of 20 male pigs were allotted to treatments of five groups of four pigs per pen. Experimental period lasted for 4 months. The nutritional composition of FFW was 56.7, 19.5 and $19.5\%$ for moisture, crude protein and ether extract, respectively. Salt content was $0.39\%$. Noxious microorganisms such as salmonella and E. coli were not detected in FFW, and contents of heavy metal and aflatoxin B1 were lower than the standard. Nutritional values of FFW pellet satisfied over $100\%$ of requirements presented in official Korean feeding standard for swine. Feeding trial for pigs showed that feed intakes were significantly (P<0.05) decreased with increasing levels of FFW pellet. T2 treatment was ideal ratio under the consideration of economical value of feeds and body weight gain of pigs. For carcass characteristics, dressing rate ($\%$) was highest in T3, and carcass grades for T2, T3 and T4 treatments were estimated as 'A'. Feed cost for FFW per kg was ${\won}167.95$, which implies $52\%$ of commercial feed cost (${\won}350/kg$). Thus, this result implied the decreased feed cost in the swine farm. Conclusively, the utilization of food wastes as feed source may lead to the reduced environmental pollution and the practice of organic livestock farming. However, our results showed that excessive amount of fermented food wastes supplementation to pigs might give rise to their reduced palatability and delayed growth.

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Decomposition of a Substituted Diphenyl Ether Herbicide(MC-4379) by Some Environmental Factors (환경요인(環境要因)에 의(依)한 치환(置換) Diphenyl Ether계(系) 제초제(除草劑) MC-4379의 분해(分解)에 관(關)한 연구(硏究))

  • Lee, Jae-Koo;Kim, Hae-Yong
    • Applied Biological Chemistry
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    • v.18 no.1
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    • pp.30-41
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    • 1975
  • A substituted diphenyl ether herbicide(MC-4379) was studied on the decomposition by some environmental factors; sunlight, microorganisms, and the crude enzyme in rice plant extract. All the decomposition products were confirmed by means of TLC, GLC, and IR. The parent compound and the decomposition products were put to the test for the effect on the growth of some plants. The results obtained are summarized as follows: 1. Photolysis Amino-MC-4379, 2,4-dichloro-3'-carboxyl-4'-nitrodiphenyl ether, Nitrofen, 2,4-dichloro-3'-carboxyl-4'-amino-diphenyl ether, amino-Nitrofen, 3-carboxymethyl-4-nitrophenol, p-nitrophenol, p-aminophenol, etc. were confirmed as photoproducts, in addition to a relatively small amount of an unknown compound. It was confirmed that the solution-phase photolysis of MC-4379 was accelerated much more by the aid of a photosensitizer benzophenone. 2. Degradation by the crude extract of germinating rice seeds Nitrofen was confirmed as a major degradation product, in addition to a relatively small amount of and unknown compound. Most of the parent compound remained unchanged. 3. Degradation by microorganisms Nitrofen and amino-MC-4379 were confirmed as the major products. in addition to a small amount of an unknown compound. 4. The germinating rice seeds and soybean were grown in the 1,000 ppm emulsions of some chemicals, respectively. The effect on rice plant growth was in the inhibitory order of p-nitrophenol > C-6989> Nitrofen > amino-Nitrofen > MC-4379. The effect on soybean was in the order of Nitrofen > amino-Nitrofen > MC-4379. Two weeds, Amantus blitum and Setaria viridis were grown in the 500 ppm emulsions containing the compounds, respectively. After incubation for 3 days, it was observed that all the shoots had been dead.

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

  • Pak, Won-Min;Do, Jung-Ah;Lim, Seung-Hee;Park, Shin-Min;Yoon, Ji-Hye;Lee, Dong-seouk;Chang, Moon-Ik
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.290-297
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    • 2017
  • The purpose of this study was developed for the determination of tridemorph in agricultural commodities samples. Tridemorph residues in samples were extracted with acetonitrile, partitioned with saline water, and then purified using and aminopropyl ($NH_2$) SPE catridge. The purified samples were quantified and confirmed via 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 (0.005~2.5 ng) into a blank extract with $r^2$ > 0.999. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. The average recovery ranged between 75.9% and 103.7% at different concentration levels (LOQ, 10 LOQ, 50 LOQ, n = 5) with relative standard deviations (RSDs) less than 9.0%. An interlaboratory study was conducted to validate the method by Korea Advanced Food Research Institute. The average recovery ranged between 87.0% and 109.2% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n = 5) with relative standard deviations (RSDs) less than 8.0%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003) and Food Safety Evaluation Department guidelines (2016). The results prove that the developed analytical methods is accurate, effective and sensitive for tridemorph determination.

Development of a Simultaneous Analytical Method for Determination of Trinexapac-ethyl and Trinexapac in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 식물생장조절제 Trinexapac-ethyl과 대사산물 Trinexapac의 동시분석법 개발)

  • Jang, Jin;Kim, Heejung;Ko, Ah-Young;Lee, Eun-Hyang;Ju, Yunji;Chang, Moon-Ik;Rhee, Gyu-Seek;Suh, Saejung
    • Korean Journal of Environmental Agriculture
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    • v.34 no.4
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    • pp.318-327
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    • 2015
  • BACKGROUND: Trinexapac-ethyl is a plant growth regulator (PGR) that inhibits the biosynthesis of plant growth hormone (gibberellin). It is used for the prevention of lodging, increasing yields of cereals, and reducing mowing of turf. The experiment was conducted to establish a determination method for trinexapac-ethyl and its metabolites trinexapac in agricultural products using LC-MS/MS.METHODS AND RESULTS: Trinexapac-ethyl and trinexapac were extracted from agricultural products with methanol/ distilled water and the extract was partitioned with dichloromethane and then detected by LC-MS/MS. Limit of detection(LOD) was 0.003 mg/kg and limit of quantification(LOQ) was 0.01 mg/kg, respectively. Matrix matched calibration curves were linear over the calibration ranges (0.01-1.0 mg/L) for all the analytes into blank extract withr2> 0.997. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, 10LOQ, 50LOQ,n=5). Recoveries of trinexapacethyl and trinexapac were within the range of 73.6-106.9%, 72.7-99.2%, respectively. The relative standard deviations (RSDs) were less than 9.0%. All values were consistent with the criteria ranges requested in the CODEX guideline(CAC/GL 40, 2003).CONCLUSION: The proposed analytical method was accurate, effective and sensitive for trinexapac-ethyl and trinexapac determination and it can be used to as an official method in Korea.

Effects of Anti-inflammation and Skin Barrier by Genistein Cyclodextrin Complex (제니스테인 Cyclodextrin 포접체의 항염 및 피부장벽에 미치는 영향)

  • Choi, Dong Jun;Cho, Uk Min;Choi, Da Hee;Hwang, Hyung Seo
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.44 no.2
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    • pp.171-181
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    • 2018
  • Genistein is one of the representative isoflavone compounds isolated from soybeans and has been studied very well for its anti-aging and anti-inflammatory activity through previous studies. However, although genistein exhibits high solubility in organic solvents, it shows low bioavaility due to the low water solubility. In this study, we compared directly the functional difference between genistein and genistein cyclodextrin complex which has the improved water solubility and stability by cell based assay. Cell cytotoxicity experiment were carried out on RAW264.7 with CCK-8 assay and cytotoxicity was appeared from $10{\mu}g/mL$, thereby maximum concentration was set to $10{\mu}g/mL$ in all condition. We discovered that genistein CD complex suppressed NO production and iNOS expression as concentration dependent manner in the condition of LPS rather than genistein. Also, we could understand that genistein CD complex was able to down-regulate mRNA expression of anti-inflammatory cytokines such as $IL1-{\alpha}$, $IL1-{\beta}$, IL-6, and $TNF-{\alpha}$ as concentration dependent manner in the presence of LPS. In addition, we verified that genistein CD complex increased TEER of HaCaT human keratinocyte cells as concentration dependent pattern and stimulated cell division and migration rather than genistein in cell migration assay. Thus, it is expected that it can be used as an effective cosmetic raw material for improving atopic dermatitis or skin barrier if clinical studies on skin regeneration and skin barrier of the genistein CD complex are carried out.