• Title/Summary/Keyword: 잔류용매

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Degradation of $^{14}C-bifenox$ in Soils under Anaerobic Conditions (혐기적 조건의 토양에서 제초제 $^{14}C-bifenox$의 분해)

  • Kwak, Hyung-Ryul;Lee, Kang-Bong;Kim, Kil-Yong;Kim, Yong-Woong;Suh, Yong-Tack
    • Korean Journal of Environmental Agriculture
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    • v.19 no.4
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    • pp.300-308
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    • 2000
  • The degradation of herbicide $^{14}C-bifenox$ was studied in soils under anaerobic conditions. $^{14}C-bifenox$ was treated in silty loam and sandy loam soils, respectively at a rate of 2.1 mg/kg, and the soil was incubated under anaerobic conditions at $25^{\circ}C$ for 180 days. The mineralization, solvent extractable and non-extractable residues, degradation products of bifenox were investigated during the experiments. The relative amounts of $^{14}CO_2$ were 1.97 and 0.9% of applied $^{14}C$ in silty loam and sandy loam soils, respectively. The non-extractable residues of sandy loam soil increased dramatically up to 79.12% of applied $^{14}C$, and were higher than those of silt loam soil, suggesting physico-chemical properties and especially organic matter contributed to the difference of $^{14}C$ between two soils. The non-extractable residues were formed mainly humin fraction and increased with time. The major metabolites were nitrofen, 5-(2,4-dichlorophenoxy)-2-Nitrobenzoate, 2,4-dichlorophenoxy aniline and methyl 5-(2,4-dichlorophenoxy) anthranilate by GC/MS analysis. From the results of volatilization, mineralization and degradation of bifenox, bifenox was stable chemically and biologically in soil.

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Improvement of Analytical Method for Residue Pesticides in Herbal Medicines Using Macroporous Diatomaceous Earth Column (다공성 규조토 컬럼을 이용한 한약재 중 잔류농약 분석법 개선)

  • Hwang, Jeong-In;Jeon, Young-Hwan;Kim, Hyo-Young;Kim, Ji-Hwan;Ahn, Ji-Woon;Seok, Da-Rong;Lee, Yoon-Jeong;Park, Ju-Young;Kim, Do-Hoon;Kim, Jang-Eok
    • The Korean Journal of Pesticide Science
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    • v.15 no.2
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    • pp.140-148
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    • 2011
  • The official analytical method of residue pesticides in herbal medicines by KFDA cannot be applied to all of the pesticides and herbal medicines because of various active materials in herbal medicines and various physicochemical properties of pesticides. Moreover, liquid-liquid partition uses harmful solvents such as methylene chloride and is consuming a lot of time and effort. In order to improve the problems, we have studied for the availability of the analytical method applying the macroporous diatomaceous earth (MDE) column instead of liquid-liquid partition to simultaneously analyze five pesticides in two dried herbal medicines. The results showed that the recovery rates of acetamiprid and azoxystrobin in Astragalus root by GC/ECD ranged from 89.6 to 94.1%, from 86.8 to 94.4%, respectively, and those of bifenthrin, chlorfenapyr, chlorpyrifos in Cnidii Rhizoma by GC/MS ranged from 83.6 to 88.4%, from 77.4 to 83.8%, from 82.6 to 84.3%, respectively. Also, the coefficients of variation (CV) for triplication ranged from 0.5 to 1.7%. The results satisfied the criteria of residue pesticide analysis, setting 70~120% for the recovery rate and below 10% for the coefficient of variation. The improved methods are safer to residue pesticide analysts, faster and less laborious than the KFDA official method.

Study on Kinetics and Thermodynamics of Rotary Evaporation of Paclitaxel for Removal of Residual Pentane (파클리탁셀의 잔류 펜탄 제거를 위한 회전증발의 동역학 및 열역학에 관한 연구)

  • Han, Jang Hoon;Ji, Seong-Bin;Kim, Ye-Sol;Lee, Seung-Hyun;Park, Seo-Hui;Kim, Jin-Hyun
    • Korean Chemical Engineering Research
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    • v.55 no.6
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    • pp.807-815
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    • 2017
  • This study investigated the removal efficiency of residual pentane from paclitaxel according to the drying temperature in the case of rotary evaporation, and performed a kinetic and thermodynamic analysis of the drying process. At all the temperatures (25, 30, 35, 40, and $45^{\circ}C$), a large amount of the residual solvent was initially removed during the drying, and the drying efficiency increased when increasing the drying temperature. Five drying models (Newton, Page, modified Page, Henderson and Pabis, Geometric) were then used for the kinetic analysis, where the Henderson and Pabis model showed the highest coefficient of determination ($r^2$) and lowest root mean square deviation (RMSD), indicating that these models were the most suitable. Furthermore, in the thermodynamic analysis of the rotary evaporation, the activation energy ($E_a$) was 4.9815 kJ/mol and the standard Gibbs free energy change (${\Delta}G^0$) was negative, whereas the standard enthalpy change (${\Delta}H^0$) and standard entropy change (${\Delta}S^0$) were both positive, indicating that the drying process was spontaneous, endothermic, and irreversible.

Analysis Method of Surfactants for Identification of Residue Dishwashing Detergent (세척제 잔류량 확인을 위한 계면활성제 분석법 확립)

  • Park, Na-Youn;Lee, Sojeong;Kim, Jung Hoan;Kho, Younglim
    • Journal of the Korean Chemical Society
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    • v.65 no.6
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    • pp.433-440
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    • 2021
  • Surfactants are organic compounds that have both hydrophilic and non-polar parts in one molecule, classified as non-ion, anion, cation, and amphoteric surfactants according to the charge of hydrophilic parts in aqueous state. A trace amounts may remain when vegetables and fruits are washed using type1 detergent (Vegetable and fruit detergent), and there is a possibility of exposure to the human body through ingestion. This study developed the simultaneous analysis method for 5 surfactants with LC-MS/MS for analysis of detergent residues after washing vegetables and fruits with detergent. The mobile phase used distilled water and acetonitrile containing 50 mM ammonium formate and 0.1% formic acid and was analyzed using a gradient method using XBridge BEH C8 column. The accuracy of the established method was 83.9-112.1%, and the precision was less than 20%. The detection limit was 7.0 (SLS) to 29.0 (SLES-N3) ㎍/L, and the correlation coefficient (r2) of calibration line regression was greater than 0.99, it is considered suitable for the analysis of trace amounts of surfactant components remaining in vegetables and fruits.

Hybrid Fabrication of Screen-printed Pb(Zr,Ti)O3 Thick Films Using a Sol-infiltration and Photosensitive Direct-patterning Technique (졸-침투와 감광성 직접-패턴 기술을 이용하여 스크린인쇄된 Pb(Zr,Ti)O3 후막의 하이브리드 제작)

  • Lee, J.-H.;Kim, T.S.;Park, H.-H.
    • Journal of the Microelectronics and Packaging Society
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    • v.22 no.4
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    • pp.83-89
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    • 2015
  • In this paper, we propose a fabrication technique for enhanced electrical properties of piezoelectric thick films with excellent patterning property using sol-infiltration and a direct-patterning process. To achieve the needs of high-density and direct-patterning at a low sintering temperature (< $850^{\circ}C$), a photosensitive lead zirconate titanate (PZT) solution was infiltrated into a screen-printed thick film. The direct-patterned PZT films were clearly formed on a locally screen-printed thick film, using a photomask and UV light. Because UV light is scattered in the screen-printed thick film of a porous powder-based structure, there are needs to optimize the photosensitive PZT sol infiltration process for obtaining the enhanced properties of PZT thick film. By optimizing the concentration of the photosensitive PZT sol, UV irradiation time, and solvent developing time, the hybrid films prepared with 0.35 M of PZT sol, 4 min of UV irradiation and 15 sec solvent developing time, showed a very dense with a large grain size at a low sintering temperature of $800^{\circ}C$. It also illustrated enhanced electrical properties (remnant polarization, $P_r$, and coercive field, $E_c$). The $P_r$ value was over four times higher than those of the screen-printed films. These films integrated on silicon wafer substrate could give a potential of applications in micro-sensors and -actuators.

Evaluation of Antimicrobial, Antithrombin, and Antioxidant Activity of Dioscorea batatas Decne (마(Dioscorea batatas Decne)의 항균, 항산화 및 항혈전 활성 평가)

  • Kim, Jee-In;Jang, Han-Su;Kim, Jong-Sik;Sohn, Ho-Yong
    • Microbiology and Biotechnology Letters
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    • v.37 no.2
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    • pp.133-139
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    • 2009
  • Yam (Dioscorea batatas Decne) has been recognized as healthy food due to its various biological activities, such as anti-obesity, anti-constipation, anti-proliferation, anti-mutagenic activity, and decrease of blood glucose and cholesterol level. In this study, the methanol extract and its organic solvent fractions were prepared from dried Dioscorea batatas Decne, and their antimicrobial, antithrombin, and antioxidant activity were evaluated, respectively. The 66.7% of methanol extract was fractioned into water residue, and most of total-polyphenol/total-flavonoids were found in ethylacetate fraction. This ethylacetate fraction at $500\;{\mu}g/disc$ concentration showed strong antibacterial activity against gram-negative and gram-positive bacteria, except Staphylococcus aureus. Antifungal activity was not observed in methanol extract and its fractions. But, strong antithrombin activity was found in methanol extract. At 4.8 mg/mL concentration, thrombin time was 99.5 sec, which is coincides with 30% activity of aspirin, a commercial available antithrombosis agent. The ethylacetate fraction showed strong DPPH scavenging activity ($IC_{50}$ of $80.5\;{\mu}g/mL$), compared to vitamin C ($IC_{50}$ of $15.2\;{\mu}g/mL$). Also, the ethylacetate fraction showed strong SOD-like activity and reducing power, which are coincide with 43% of vitamin C and 82.7% of butylated hydroxytoluene activity, respectively.

Development of Method for Analysis of Four Sulfonylurea Pesticides, Rimsulfuron, Ethametsulfuron-methyl, Tribenuron-methyl, Chlorimuron-ethyl Residues by High-Performance Liquid Chromatography with Diode-Array Detection (HPLC/DAD를 이용한 림술푸론, 에타메트설푸론메틸, 트리베누론메칠, 클로리무론에칠 4종 성분의 잔류농약 분석법 개발)

  • Koo, Yun-Chang;Yang, Sung-Yong;Wang, Zeng;An, Eun-Mi;Heo, Kyoung;Kim, Hyeng-Kook;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.1231-1235
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    • 2010
  • The method for residue analysis of four sulfonylurea pesticides, rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl and chlorimuron-ethyl was examined and analyzed by HPLC with ODS column ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$ diameter particle size) which was maintained at $35^{\circ}C$. Mobile phase consisted of solvent A (20 mM $KH_2PO_4$, pH 2.5) and solvent B (acetonitrile). Isocratic elution of the column with 45% solvent A and 55% solvent B at a flow rate of 1 mL/min resulted in retention times of 5.92, 6.54, 9.28, and 14.35 min for rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl, and chlorimuron-ethyl, respectively. All injection volumes were $20\;{\mu}L$. The limit of quantitation was 0.02, 0.01, 0.001, and 0.004 mg/kg for rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl, and chlorimuron-ethyl, respectively. Recovery rate test was performed with three farm products, rice, apple and soybean. Four sulfonylurea pesticides were spiked at concentrations of 0.05, 0.1 and 0.5 mg/kg. The recovery rates were ranged from 86.12% to 116.26% and the standard deviations of all experiments were within 10%.

Anti-thrombosis and anti-oxidative activity of the root of Arctium lappa L. (우엉 뿌리의 항혈전 및 항산화 활성)

  • Kim, Mi-Sun;Lee, Ye-Seul;Sohn, Ho-Yong
    • Food Science and Preservation
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    • v.21 no.5
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    • pp.727-734
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    • 2014
  • To investigate anti-thrombosis and anti-oxidation activities of the root of Arctium lappa L (RALL), which has been used as foodstuff and oriental medicine in Korea, the ethanol extract and its subsequent organic solvent fractions of the RALL were prepared. The yield of ethanol extraction was 10.94%, and the content of total polyphenol and total sugar of ethanol extract were 5.01 and 694.53 mg/g, respectively. The fraction yields of n-hexane, ethylacetate (EA), butanol and water residue were 1.62, 0.42, 5.98 and 85.38%, respectively. In anticoagulation activity assay, the ethanol extract of RALL did not show significant changes in thrombin time (TT), prothrombin time (PT) and activated partial thromboplastin time (aPTT), whereas the EA fractions showed 13 folds extended TT, PT, and aPTT respectively. Interestingly, the water residue showed strong activation effect against blood clotting factors with shortened aPTT, which might provide the evidence of coagulation agent of RALL in folk remedy. In anti-platelet aggregation assay, the activity of the ethanol extract and its fractions were comparable to that of aspirin. Especially the EA fraction showed 2-folds higher inhibitory activity than aspirin. In anti-oxidation activity assay, the EA fraction also showed strong in DPPH, ABTS and nitrite scavenging activity, and reducing power activity. The extract and fractions of RALL have ignorable hemolytic activity against human RBC up to 0.5 mg/mL concentration. Our results suggest that the EA fraction of RALL have potentials as safe and novel anti-thrombosis agent.

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.

A study on the Separation of Acetic Acid, Nitric Acid and Hydrofluoric Acid from Waste Etching Solution of Si Wafer Manufacturing Process (Silicon wafer 에칭공정시 발생(發生)되는 폐(廢)에칭액 으로부터 초산(醋酸), 질산(窒酸) 및 불산(弗酸)의 분리.회수(分離.回收)에 관한 연구(硏究))

  • Kim, Jun-Young;Lee, Hyang-Sook;Shin, Chang-Hoon;Kim, Ju-Yup;Kim, Hyun-Sang;Ahn, Jae-Woo
    • Resources Recycling
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    • v.16 no.1 s.75
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    • pp.59-67
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    • 2007
  • Recovery of acids from the waste etching solution of containing acetic, nitric and hydrofluoric acid discharged from silicon wafer manufacturing process has been attempted by using solvent extraction method. EHA(2-Ethylhexlalcohol) for acetic acid and TBP(Tri-butly Phosphate) for nitric and hydrofluoric acid as a extraction agent was used to the experiment to obtain the process design data in separation procedure. From the experimental data and McCabe-Thiele diagram analysis, we obtained the optimum conditions of phase ratio(O/A) and stages to separate each acid sequently from the mixed acids. The recovery yield was obtained above 90% for acetic acid from the acid mixtures, 90% for nitric acid from acetic acid extraction raffinate and then above 67% for hydrofluoric acid from final extraction raffinate.