• Title/Summary/Keyword: Residue analysis

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Establishment of an Analytical Method for Determination of Fungicide Oxathiapiprolin in Agricultural Commodities using HPLC-UV Detector (HPLC-UVD를 이용한 농산물 중 살균제 Oxathiapiprolin의 잔류분석법 확립)

  • Jang, Jin;Kim, Heejung;Do, Jung Ah;Ko, Ah-Young;Lee, Eun Hyang;Ju, Yunji;Kim, Eunju;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.31 no.3
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    • pp.186-193
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    • 2016
  • An analytical method was developed for the determination of oxathiapiprolin in agricultural commodities. Oxathiapiprolin is a new oomycide (fungicide of piperidinyl thiazole isoxazoline class) which controls downy mildew in cucurbits caused by Pseudoperonospora cubensis (oomycete plant pathogen). Agricultural commodities were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, adjusting pH between 9 and 10 by 1 N sodium hydroxide. After purification by silica SPE cartridge to clean up the interference of organic compounds, they were finally quantified by HPLC-UVD (high performance liquid chromatograph ultraviolet detector) using a wavelength at 260 nm and confirmed by LC-MS (liquid chromatograph mass spectrometer) in electro-spray ionization positive ion mode. The standard calibration curve was linear with coefficients of determination ($r^2$) 1.00 over the calibration ranges (0.025-2.5 mg/L). Recoveries were ranged between 86.7 to 112.7%, with relative standard deviations less than 10% at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates. The overall results were determined and estimated according to the CODEX guidelines (CAC/GL40). The proposed method for determination of oxathiapiprolin residues in agricultural commodities can be used as an official method.

Analysis of Four Pesticides, Isoproturon, Phenmedipham, Pyridate and Nitenpyram Residues by High-Performance Liquid Chromatography with Diode-Array Detector (HPLC를 이용한 Isoproturon, Phenmedipham, Pyridate 및 Nitenpyram 4종 성분의 잔류농약 분석법 개발)

  • Yang, Sung-Yong;Koo, Yun-Chang;Wang, Zeng;Heo, Kyeong;Kim, Hyeong-Kook;An, Eun-Mi;Shin, Han-Seung;Lee, Jin-Won;Lee, Kwang-Won
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.39 no.8
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    • pp.1165-1170
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    • 2010
  • A method for the determination of four pesticide compounds, urea (isoproturon), bis-carbamate (phenmedipham), thiocarbamate (pyridate) and vinyllidenediamine (nitenpyram) were examined and analyzed by HPLC with C-18 column ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$ diameter particle size). Mobile phase consisted of deionized water, acetonitrile and 50 mM $KH_2PO_4$ (pH 2.5). Isoproturon and phenmedipham analytical condition was isocratic elution of the column with 50% solvent A (acetonitrile) and 50% solvent B (deionized water); pyridate was 85% solvent A (acetonitrile) and 15% solvent B (deionized water) at a flow rate of 1 mL/min; and nitenpyram analytical condition was 90% solvent A (50 mM $KH_2PO_4$, pH 2.5) and 10% solvent B (acetonitrile) at a flow rate of 1 mL/min. In results, retention times were 6.12, 8.63, 9.40 and 12.76 min for isoproturon, phenmedipham, pyridate and nitenpyram, respectively. All injection volumes were $10\;{\mu}L$ and the limit of quantitation was 0.05 mg/kg for four pesticide compounds, respectively. Recovery rate test was performed with three farm products, rice, apple and soybean. Four pesticide compounds were spiked at concentrations of 0.05, 0.1 and 0.5 mg/kg. The recovery rates were ranged from 70.18% to 118.08% and the standard deviations of all experiments were within 10%.

Removals of 1-Naphthol in Aqueous Solution Using Alginate Gel Beads with Entrapped Birnessites (버네사이트를 고정화한 알긴산 비드(Bir-AB)를 이용한 수용액 중 1-Naphthol의 제거)

  • Eom, Won-Suk;Lee, Doo-Hee;Shin, Hyun-Sang
    • Journal of Korean Society of Environmental Engineers
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    • v.35 no.4
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    • pp.247-256
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    • 2013
  • In this study, alginate beads containing birnessite (Bir-AB), a highly reactive oxidative catalyst for the transformation of phenolic compounds, was prepared and its 1-naphthol (1-NP) removal efficiency was investigated in a batch test. Based on scanning electron microscopy image, it can be inferred that the alginate gel cluster acts as a bridge which bind the birnessite particles together. Kinetic experiment with Bir-AB of different mixing ratios of birnessite to alginate (Bir : AG=0.25 : 1~1 : 1 w/w) indicate that pseudo-first order kinetic constants, $k(hr^{-1})$ for the 1-NP removals increased about 1.5 times when the birnessite mixing ratio was doubled. The removals of 1-NP was found to be dependent on solution pH and the pesudo-first order rate constants were increased from 0.331 $hr^{-1}$ at pH 10 to 0.661 $hr^{-1}$ at pH 4. The analysis of total organic carbon for the reaction solutions showed that a higher removal of dissolved organic carbon was achieved with Bir-AB as compared to birnessite. HPLC chromatographic analysis of the methanol extract after reaction of 1-NP with Bir-AB suggest that the reaction products could be removed through incorporation into the aliginate beads as a bound residue. Mn ions produced from the oxidative transformation of 1-NP by birnessite were also removed by sorption to Bir-AB. The Bir-AB was recovered quantitatively by simple filtration and was reused twice without significant loss of the initial reactivity.

Reliability of a Cobalt Silicide on Counter Electrodes for Dye Sensitized Solar Cells (코발트실리사이드를 이용한 염료감응형 태양전지 상대전극의 신뢰성 평가)

  • Kim, Kwangbae;Park, Taeyeul;Song, Ohsung
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.18 no.4
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    • pp.1-7
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    • 2017
  • Cobalt silicide was used as a counter electrode in order to confirm its reliability in dye-sensitized solar cell (DSSC) devices. 100 nm-Co/300 nm-Si/quartz was formed by an evaporator and cobalt silicide was formed by vacuum heat treatment at $700^{\circ}C$ for 60 min to form approximately 350 nm-CoSi. This process was followed by etching in $80^{\circ}C$-30% $H_2SO_4$ to remove the cobalt residue on the cobalt silicide surface. Also, for the comparison against Pt, we prepared a 100 nm-Pt/glass counter electrode. Cobalt silicide was used for the counter electrode in order to confirm its reliability in DSSC devices and maintained for 0, 168, 336, 504, 672, and 840 hours at $80^{\circ}C$. The photovoltaic properties of the DSSCs employing cobalt silicide were confirmed by using a simulator and potentiostat. Cyclic-voltammetry, field emission scanning electron microscopy, focused ion beam scanning electron microscopy, and energy dispersive spectrometry analyses were used to confirm the catalytic activity, microstructure, and composition, respectively. The energy conversion efficiency (ECE) as a function of time and ECE of the DSSC with Pt and CoSi counter electrodes were maintained for 504 hours. However, after 672 hours, the ECEs decreased to a half of their initial values. The results of the catalytic activity analysis showed that the catalytic activities of the Pt and CoSi counter electrodes decreased to 64% and 57% of their initial values, respectively(after 840 hours). The microstructure analysis showed that the CoSi layer improved the durability in the electrolyte, but because the stress concentrates on the contact surface between the lower quartz substrate and the CoSi layer, cracks are formed locally and flaking occurs. Thus, deterioration occurs due to the residual stress built up during the silicidation of the CoSi counter electrode, so it is necessary to take measures against these residual stresses, in order to ensure the reliability of the electrode.

Effects of Vitamin C on Residual Aflatoxin $B_1$ in Rat Sera Treated with Radiation and Aflatoxin $B_1$ (Vitamin C가 방사선과 Aflatoxin $B_1$을 투여한 흰쥐의 혈청 중 Aflatoxin $B_1$ 잔류량에 미치는 영향)

  • Chung, Do-Young;Kim, Han-Soo;Kang, Jin-Soon
    • Food Science and Preservation
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    • v.18 no.3
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    • pp.374-382
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    • 2011
  • Aflatoxin ($AFB_1$) is a potent hepatotoxic and hepatocarcinogenic mycotoxin in humans. It is also well-known to be accumulated in animal tissues via various metabolic pathways. This study was conducted to determine the effects of vitamin C on the residual $AFB_1$ in rat sera that were treated with radiation and $AFB_1$. Six week-old male Sprague-Dawley rats were randomly divided into five groups: a control group, $AFB_1$-treated group, the group treated with $AFB_1$ and vitamin C, the group treated with X-ray and AFB1, and the group treated with X-ray and $AFB_1$ with vitamin C. On the first day of the experiment, only one dose of X-rays was exposed to the entire liver at 1,500 cGy. Next, vitamin C was injected at 10 mg/kg body weight via intraperitoneal injection, followed 1 hr later by the administration of 0.4 mg/kg of $AFB_1$ via intraperitoneal injection. These treatments were then administered every three days over a period of 15 days. On the 16th day of treatments, the animals were sacrificed. The contents of $AFB_1$ in rat sera were determined via indirect competitive ELISA and HPLC method. In the quantitative analysis of $AFB_1$ in rat sera via ELISA, $5.17{\pm}0.34$ ng/mL of $AFB_1$ was detected in the $AFB_1$-treated groups, but the amount more significantly decreased to $3.23{\pm}0.76$ ng/mL in the groups treated with $AFB_1$ and vitamin C (p<0.01) than in the $AFB_1$-treated groups. The $AFB_1$ contents of the rat sera of the groups treated with X-ray and $AFB_1$ did not significantly decreased with the administration of vitamin C. The $AFB_1$ content of the rat sera that was analyzed via HPLC showed a tendency similar to that of the content that was analyzed via ELISA. With regard to these data, vitamin C was very effective in reducing $AFB_1$ residue in rat sera.

Monitoring of Pesticide Residues on Herbs and Spices (향신식물의 잔류농약 실태조사)

  • Bae, Ho-Jeong;Kim, Woon-Ho;Jung, You-Jung;Lee, Yu-Na;Moon, Kyeong-Eun;Kim, Jung-Sun;Chae, Kyung-Suk;Lee, Jin-Hee;Do, Young-Sook;Choi, Ok-Kyung
    • Journal of Food Hygiene and Safety
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    • v.36 no.5
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    • pp.392-399
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    • 2021
  • This study was conducted to research the status of pesticide residues in a total of 114 herbs and spices obtained from January to October 2020. 341 pesticide residues were analyzed by the multi class pesticide multiresidue methods using GC-MSMS, GC-ECD, GC-NPD, LC-MSMS, LC-PDA, and LC-CAS. As a result of analysis, 36 pesticide residues were found, and detection rate was 31.6%. Of them, seven samples were detected over Maximum Residue Limits (MRLs) and the unsuitable level in pesticide was 6.1%. The herbs and spices exceeding MRLs include coriander (2 times), mint (2 times), basil (once), rosemary (once), and boraye (once). According to an analysis of 341 pesticide residues, 22 pesticides were detected 52 times and 8 pesticides were found to exceed the MRLs. The pesticides exceeding MRLs were ingredients such as etofenprox, flufenoxuron, fluquinconazole, iprodione, lufenuron, paclobutrazol, phenthoate, and spiromesifen.

Estimation of Food Commodity Intakes from the Korea National Health and Nutrition Examination Survey Databases: With Priority Given to Intake of Perilla Leaf (국민건강영양조사 자료를 이용한 식품 섭취량 산출 방법 개발: 들깻잎 섭취량을 중심으로)

  • Kim, Seung Won;Jung, Junho;Lee, Joong-Keun;Woo, Hee Dong;Im, Moo-Hyeog;Park, Young Sig;Ko, Sanghoon
    • Food Engineering Progress
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    • v.14 no.4
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    • pp.307-315
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    • 2010
  • The safety and security of food supply should be one of the primary responsibilities of any government. Estimation of nation's food commodity intakes is important to control the potential risks in food systems since food hazards are often associated with quality and safety of food commodities. The food intake databases provided by Korea National Health and Nutrition Examination Survey (KNHANES) are good resources to estimate the demographic data of intakes of various food commodities. A limitation of the KNHANES databases, however, is that the food intakes surveyed are not based on commodities but ingredients and their mixtures. In this study, reasonable calculation strategies were applied to convert the food intakes of the ingredients mixtures from the KNHANES into food commodity intakes. For example, Perilla leaf consumed with meat, raw fish, and etc. in Korean diets was used to estimate its Korean intakes and develop algorithms for demographic analysis. Koreans have consumed raw, blanched, steamed, and canned perilla leaf products. The average daily intakes of the perilla leaf were analyzed demographically, for examples, the intakes by gender, age, and etc. The average daily intakes of total perilla leaf were 2.03${\pm}$0.27 g in 1998, 2.11${\pm}$0.26 g in 2001, 2.29${\pm}$0.27 g in 2005, 2.75${\pm}$0.35 g in 2007, and 2.27${\pm}$0.20 g in 2008. Generally, people equal to or over 20 years of age have shown higher perilla leaf intakes than people below 20. This study would be contributed to the estimation of intakes of possible chemical contaminants such as residual pesticides and subsequent analysis for their potential risk.

Investigation of Food Safety Attitude, Knowledge, and Behavior in College Students in Gyeonggi Region (경기도 지역 대학생의 식품 안전성에 대한 태도와 지식 및 행동 분석)

  • Kim, Ji-Myung;Hong, Seung-Hee
    • Journal of Food Hygiene and Safety
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    • v.33 no.6
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    • pp.438-446
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    • 2018
  • The purpose of this study was to investigate food safety awareness, knowledge, and behavior in college students, to provide basic data for the increase in food safety awareness. Data were collected from 252 college students in Gyeonggi region, using a self-administered questionnaire. In results of concern about food safety, subjects responded 3.48 of 5.00 and have knowledge about food safety education revealing significantly higher awareness and concern than subjects without knowledge about food safety education. Food safety awareness of distributed food was 2.55, considered unsafe. Among reasons in perceiving food as unsafe, 62.3% of subjects expressed distrust about safety relative food production. As for risk factors relative to food safety, subjects responded that the highest risk factor was food additives (2.35), followed by heavy metal (2.38) and endocrine disrupters (2.38). Correlation analysis resulting in risk factors for food had positive correlation with each other, heavy metal revealed highest correlation with pesticide residue (r = 0.674), than with endocrine disrupters (r = 0.672). Also, genetically modified food revealed high correlation with radiation irradiated food. Regression analysis demonstrated that concern about food safety significantly influenced pro-actively engaging in food safety education. Meanwhile, 63.5% of subjects correctly responded to food safety knowledge items. The item 'the heavy metals are contaminated the most, in the roots of vegetables' revealed the lowest correct answer rate (38.1%). In food safety behavior, the item 'always wash hands before handling food and meal's revealed 3.85, and subjects with awareness and concern about food safety education, responded in significantly higher numbers than subject without awareness and concern about food safety. The most neglected concern was relative to frozen food thawed at room temperature. Together, students recognize that distributed foods are unsafe, and students with awareness and concern about food safety education showed higher knowledge compared to without awareness and concern experience about food safety eduction. So, systematic education using accurate and objective data is required to reduce anxiety and raise the level of awareness and concern about food safety.

Changes of Monosaccharides Contents in Hydrolysates of Decomposing Plant Residues (식물성(植物性) 유기물질(有機物質)의 부숙과정중(腐熟過程中) 단당류(單糖類)의 함량(含量) 변화(變化))

  • Kim, Jeong-Je;Jang, Yong-Seon;Shin, Young-Oh
    • Korean Journal of Soil Science and Fertilizer
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    • v.23 no.1
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    • pp.21-25
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    • 1990
  • The amounts of monosaccharides in acid hydrolysates of decomposing plant residues under laboratory conditions were determined. Straw of cereal rice and barley, wild grass cutting, and litters of deciduous and coniferous forest trees were treated to decompose for 90 days. Samples for the analysis of mono-saccharides were taken at 3 different periods of incubation. 1. Fractions of monosaccahrides in plant residues steadily decreased with the time of decomposition. In some samples there appeared an intermediate stages where the fractions reached the highest level. 2. Decomposition of barley straw occured at a faster rate than that of rice straw, and so did the decomposition of deciduous litter than that of coniferous litter. 3. Cereal crop residues of rice and barley were richer in monosaccharides than residues of wild grass cutting and forest litters. 4. Distiction between monosaccharides of plant origin and those of microbial origin was not possible to make in this study. 5. Glucose was the predominent monosaccharide and fucose was the monosaccharide contained in the smallest amount. No measurable ribose was detected from any sample. 6. The relative proportion of galactose in creased with the time of incubation. 7. In general, the proportion of fucose decreased with time and so did that of rhamnose, rhamnose of rice straw residue being the exception. 8. The orders of abundance of monosaccharides after decomposition of 90 days were as the following: in rice straw; glucose > xylose > arabinose > galactose > rhamnose > mannose > fucose, in barley straw; glucose > xylose > arabinose > galactose> mannose > rhamnose > fucose, in wild grass cutting; glucose > xylose > galactose arabinose> rhamnose mannose > fucose, in deciduous litter; glucose > arabinose > xylose galactose > mannose > rhamnose = fucose, and in coniferous litter; glucose > xylose > galactose > arabinose mannose > rhamnose > fucose.

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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.