• Title/Summary/Keyword: 표준시료

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Operator Exposure to Indoxacarb Wettable Powder and Water Dispersible Granule during Mixing/loading and Risk Assessment (Indoxacarb의 수화제 및 입상수화제 살포액 조제 시 농작업자의 노출량 측정 및 위해성 평가)

  • Kim, Eunhye;Hwang, Yon-Jin;Kim, Suhee;Lee, Hyeri;Hong, Soonsung;Park, Kyung-Hun;Kim, Jeong-Han
    • The Korean Journal of Pesticide Science
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    • v.16 no.4
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    • pp.343-349
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    • 2012
  • Exposure and risk assessments were conducted to evaluate the relative safety of mixing/loading work of indoxacarb between wettable powder (WP) and water dispersible granule (WG). Hand exposure was monitored using cotton gloves while inhalation exposure was measured using personal air monitor. Method validation for the exposure monitoring was established successfully through several experiments. Limit of determination and limit of quantitation were 0.25 and 1 ng, respectively. $R^2$ of calibration curve linearity was more than 0.9999 and reproducibility was 0.7-6. Recovery of indoxacarb from gloves, solid sorbent and glass fiber filter at three different levels was 81.5-108.8%. Trapping efficiency and breakthrough tests gave 981.5-108.8% of recovery. During mixing/loading procedure, hand exposure amount (75 percentile of 30 repetitions) for indoxacarb WP was 6 folds (459.8 mg/kg a.i) than that of WG (81.4 mg/kg a.i). This result indicates that WG has less drift than WP thanks to its granular type of formulation. Inhalation amount was $10^{-8}-10^{-7}%$ of spray mixture prepared and $10^{-4}-10^{-3}%$ of hand exposure. In inhalation case, no significant differences were observed between two formulations. Margin of safety was calculated for risk assessment using male Korean average body weight and acceptable operator exposure level as the important exposure factors. Mixing/loading procedures for both of the formulations were considered to be of least risk because calculated MOS values were more than 1.

Establishment of Pre-Harvest Residue Limits and Residue Characteristics of Penthiopyrad and Pyriofenone in Cucumber (Cucumis sativus L.) Under Greenhouse Condition (시설 내 오이(Cucumis sativus L.) Penthiopyrad 재배 중 및 Pyriofenone의 잔류특성과 생산단계 잔류허용기준 설정)

  • Leem, Su-Bin;Kim, Ji-Yoon;Hur, Kyung-Jin;Kim, Hee-Gon;Hur, Jang-Hyun
    • Korean Journal of Environmental Agriculture
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    • v.36 no.1
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    • pp.43-49
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    • 2017
  • BACKGROUND: Greenhouse crops are one of agricultural products consumed largely in Korea. Cucumber is a typical example as main vegetables of greenhouse crops. Thus, pesticide residue analysis is an important requirement to guarantee pesticide safety of cucumber. This work was aim to investigate the residues of penthiopyrad and pyriofenone in cucumber after harvest. METHODS AND RESULTS: Cucumber was subjected to treat with penthiopyrad and pyriofenone at a level of recommended dose 0, 1, 2, 3, 5, 7 and 10 days before harvest under greenhouse conditions. The samples were extracted with organic solvent by using a homogenizer and purified on solid phase cartridge column followed by LC-MS/MS analysis. The recovery levels of penthiopyrad and pyriofenoneranged from approximately 81 to 93% with the method limit of 0.005 mg/kg and coefficient of variation less than 10%. Penthiopyrad and pyriofenone were detected at a level less than maximum residue limit in cucumber at 10 days before. The half-lives of penthiopyrad and pyriofenone were determined to 2.4 ~ 2.6 days. CONCLUSION: Penthiopyrad and pyriofenone are suggested to use in cucumber 10 days before harvest to reach their levels less than maximum residue limit.

Monitoring of Forbidden Medicines as Adulterants in Dietary Supplements Marketed Online by HPLC and ESI-tandom Mass Spectrometry (HPLC 및 ESI-tandom Mass Spectrometry를 이용한 인터넷에서 판매되는 기능성표방식품 중 부정유해물질 모니터링)

  • Lee, Yong-Cheol;Kim, Bog-Soon;Yun, Eun-Sun;Kim, Sung-Dan;Chang, Min-Su;Park, Young-Ae;Shin, Young;Jung, Sun-Ok;Lee, Jae-In;Chae, Young-Zoo
    • Korean Journal of Food Science and Technology
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    • v.44 no.2
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    • pp.148-154
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    • 2012
  • It was carried out to detect anti-impotence drug-like compounds, sibutramine and their analogues in dietary supplements, which are doubtful whether they include illegal compounds. A total of 51 food products were bought online and have been investigated. The separation was achieved on a C18 column, with the mobile phase made up of water (5 mM sodium hexanesulfonate and 0.1% phosphoric acid) and 95% acetonitrile, at a flow rate of 1.2 mL/min with gradient elution using by HPLC-DAD. The UV signals were monitored at 220 nm and 291 nm. LC-ESI-tandom MS was utilized to confirm that detected compounds in samples are the same as the reference materials. Two nutrient supplement foods and ginseng products were found to contain 1.3-82.1 mg of sildenafil, dimethylthiolsildenafil and pseudovardenafil per serving size. In addition, two other processed products were detected to contain 1.7 and 2.2 mg of didesmethylsibutramine, derived from sibutramine per serving size.

Boulangerite from the Janggun Mine, Republic of Korea; Contributions to the Knowledge of Ore-Forming Minerals in the Janggun Lead-Zinc-Silver Ores (2) (한국·장군광산산 보울란저라이트에 대하여; 장군 연·아연·은 구성광물의 지식에 대한 기여 (2))

  • Lee, Hyun Koo;Imai, Naoya
    • Economic and Environmental Geology
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    • v.26 no.2
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    • pp.129-134
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    • 1993
  • At the Janggun mine, boulangerite usually occurs as needles or irregularly-shaped grains, up to $500{{\mu}m}$ in longer dimensions, closely associated with galena, minerals of a tetrahedrite-freibergite series and bournonite in the peripheries of South A and B orebodies and the zone of manganoan carbonates surrounding them. In some places, especially at the top of South B orebody, it occures as "feather ore" consisting of its fine needles or "hairs" in small drusy cavities together with fine-grained euhedral galena, pyrite, manganoan carbonates, quartz, etc. In reflected light, it is bluish grey in colour exhibiting moderate bireflectance and is strongly anisotropic without any internal reflections. Reflectance in air is $R_{max}=43.2$, $R_{min}=35.7$ percent at wavelength of 580 nm, and VHN: $146-173\;kg/mm^2$ at a 50 g-load. The chemical composition on the average from 23 complete spot analyses by electron microprobe is, Pb 56.1, Sb 25.1, S 18.5, Total 99.6 (all in weight percent); the corresponding chemical formula calculated on the basis of S=11 is; $Pb_{5.16}Sb_{3.93}S_{11.0}$ which fulfils approximately the ideal formula $Pb_5Sb_4S_{11}$. The strongest reflections on the X-ray diffraction pattern are; $3.73\;{\AA}\;(10)$, $3.22\;{\AA}\;(5)$, $3.03\;{\AA}\;(4)$ and $2.82\;{\AA}\;(5)$ and the pattern is in harmonic with space group $C^5_{2h}-P2_1/a$. From the textural evidence of the microscopic observations, the mineral is considered to have been formed at the latest stage of hydrothermal lead-zinc-silver mineralization.

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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.

Evaluation of the Efficiency of E. coli O157: H7 Rapid Detection Kit using Immunochromatography (면역크로마토그래피를 이용한 E. coli O157: H7 신속검출 키트의 유효성 평가)

  • Kwak, Hyo-Sun;Lee, Dong-Ha;Moon, Hee-Sook;Park, Jong-Seok;Woo, Gun-Jo;Kim, Chang-Min
    • Journal of Food Hygiene and Safety
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    • v.18 no.3
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    • pp.118-124
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    • 2003
  • For the rapid detection of various pathogenic microorganisms from food sample, various kinds of kits have been developed and commercially available in the markets. With the advantages of speed, accuracy and easiness, the market of these kits has gradually increased for the QC and QA field of food company as well as testing facilities or laboratories. In this study, the characteristics such as the detection limit and the sensitivity of immunochromatographic type of rapid detection kit (Donga Co, Korea, D-kit) for E. coli 0157:H7 developed by monoclonal antibody were examined and also the possibility of application of the kit to food samples was evaluated. The reference kits used for comparison study were Reveal E. coli 0157:H7 (Neogen Co., USA, R-kit) and VIP EHEC kit (Biocontrol Inc., USA, V-kit) occupying major market share. In the detection limit test with the E. coli 0157:H7 reference, both R-kit and D-kit showed a distinct positive reaction in $10^4$/ml and weak positive reaction in $10^3$/ml, whereas V-kit showed a same reaction in 105/ml. Also, it was identified that the culture treated with heat showed more sensitivity than no heat treated culture. The sensitivity test was conducted against 22 isolates of E. coli 0157:H7, 7 strains of non-O157:H7 verotoxin-producing E. coli, 40 strains of E. coli with different O and H antigen type, and 38 strains of non-E. coli Enterobacteriaceae, and all of the test strains except three were showed exactly three were showed exactly the same reaction against three kinds of the tested kits. All the three kinds of kits showed a positive reaction against E. coli O157:H19, E. coli O148:H18 and Salmonella galinarium. We suppose that there might be a similarity in serological property between these three strains and O157:H7. From the test results, it can be concluded that there is (was) no difference between the D-kit developed in this study and R-kit or V-kit based on the detection limit and sensitivity.

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.

Development and Validation of the Determination of Sorafenib in Human Plasma using Tandem Mass Spectrometry Coupled with Liquid Chromatography (고속액체크로마토그래피 텐덤질량분석기법을 이용한 사람 혈장 내 소라페닙 농도분석법의 개발 및 검정)

  • Park, Daejin;Lee, Sunggon;Kim, Woomi
    • Journal of Life Science
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    • v.22 no.11
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    • pp.1456-1462
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    • 2012
  • Sorafenib is a multikinase inhibitor and an oral anticancer drug approved for the treatment of patients with advanced renal cell carcinoma and those with unresectable hepatocellular carcinoma. The purpose of this study was to develop an efficient method of the determination of sorafenib in human plasma using tandem mass spectrometry coupled with liquid chromatography (LC/MS/MS) and validate the method by the guidelines of the Korean Food and Drug Administration (KFDA). Plasma samples ($100{\mu}l$) were added with chlorantraniliprole as an internal standard and then mixed with the 0.1% formic acid-containing extraction solution composed of isopropyl alcohol and ethyl acetate (1:4, v/v). After centrifugation, the supernatant was concentrated at $45^{\circ}C$ under negative pressure and centrifugal force. The residue was reconstituted with a mobile phase and injected into the HPLC instrument using a reverse phase Waters XTerra$^{TM}$ C18 column (particle size $3.5{\mu}m$). Liquid chromatography was carried out within the run time of 5 min using a mobile phase composed of buffer (0.1% formic acid and 10 mM ammonium formate), methanol, and acetonitrile (1:6:3, v/v/v). The analytes were monitored by tandem mass spectrometry in the multiple reaction monitoring method programmed to detect sorafenib at 'm/z 465.2 ${\rightarrow}$ 252.5' and chlorantraniliprole at 'm/z 484.4 ${\rightarrow}$ 286.2' with positive electrospray ionization mode ($ES^+$). The result showed the proper linearity ($r^2$ > 0.99) over the range of 2,000-5,000 ng/ml with good accuracy (90.7-103.9%) and precision (less than 10%). The newly developed method using LC/MS/MS was validated by the guideline of KFDA and identified as more sensitive compared to the previous methods.

Effect of Supplementation of Korean Native Chicken Egg Fed with Citrus Peel on Profiles in Sprague-Dawley Rats (감귤 껍질을 급여한 토종닭 계란이 흰쥐의 혈액 성상에 미치는 영향)

  • Moon, Yoon-Hee;Yang, Jong-Beom;Jung, In-Chul
    • Journal of the East Asian Society of Dietary Life
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    • v.19 no.4
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    • pp.579-584
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    • 2009
  • In this experiment, three different diets were produced to investigate the effects of Jeju native chicken eggs fed with citrus peel on the profiles of rats. The first diet did not contain any eggs (TS), the second diet contained 10% eggs and no citrus peels (T0), and the third diet contained 10% chicken egg with citrus peels (T1). These diets were provided to 11-week-old male rats for four weeks. The weight gain, feed intake and feed efficiency were not significantly different between the three treatment groups, TS, T0, and T1. The weight of the liver was significantly higher in T0 and T1 than TS (p<0.05), but the weights of the kidney and epididymal fat pad were not significantly different between the TS, T0, and T1 groups. The total lipid, phospholipid, triglycerides, total cholesterol and LDL cholesterol did not significantly difference among the TS, T0, and T1 groups. The HDL cholesterol and HDL cholesterol/ total cholesterol of T1 were the highest among the groups, and the atherogenic index of T1 was the lowest among the groups (p<0.05). The total protein of TS was significantly lower in T0 and T1, and the albumin of T1 was the highest among the groups (p<0.05). The albumin/globulin ratio of TS was significantly higher in T0 and T1, but the creatinine of T0 was significantly higher in T0 and T1 (p<0.05). The blood sugar and blood pigment were not significantly different between the TS, T0, and T1 groups. The $\gamma$-GTP of T1 was the lowest among the groups (p<0.05), but the ALT, AST and ALP did not show significant difference among the TS, T0, and T1 groups.

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Effects of different cooking methods on folate retention in selected mushrooms (다양한 조리법에 따른 버섯류의 엽산 리텐션)

  • Park, Su-Jin;Park, Sun-Hye;Chung, Heajung;Lee, Junsoo;Hyun, Taisun;Chun, Jiyeon
    • Food Science and Preservation
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    • v.24 no.8
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    • pp.1103-1112
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    • 2017
  • This study was performed to investigate the effects of different cooking methods (boiling, roasting, stir-frying, and deep-frying) on folate retention in 6 kinds of mushrooms (Beech-, button-, Juda's ear-, oak-, oyster-, and winter-mushrooms) frequently consumed in Korea. In order to assure reliability of analytical data, trienzyme extraction-L casei method was verified and analytical quality control was also evaluated. Folate contents of mushrooms varied by 6.04-64.82 g/100 g depending on the type of mushrooms. and were significantly affected by cooking methods. Depending on cooking methods, folate contents of mushrooms decreased by 22-48%, 2-31%, and 17-56% for Juda's ear-, oak- and oyster-mushrooms, respectively, while 17-90% of folate was increased in Beech mushroom. Overall, the largest weight loss was found in boiled mushrooms, but the lowest one in deep-fried samples. True folate retention rates considering processing factor were less than 100% for all cooked mushrooms except for Beech samples. Overall, folate loss was the largest by boiling with water but the smallest by deep-frying. Both accuracy and precision of trienzyme extraction-L-casei method were excellent based on a recovery close to 100% and coefficient variations less than 3%. Quality control chart of folate analysis (n=26) obtained during the entire study and an international proficiency test (z-score=-0.5) showed that trienzyme extraction-L casei method is reliable enough for production of national folate database.