• Title/Summary/Keyword: Relative Interference

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Improvement of analytical methods for arsenic in soil using ICP-AES (ICP-AES를 이용한 토양 시료 중 비소 분석 방법 개선)

  • Lee, Hong-gil;Kim, Ji In;Kim, Rog-young;Ko, Hyungwook;Kim, Tae Seung;Yoon, Jeong Ki
    • Analytical Science and Technology
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    • v.28 no.6
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    • pp.409-416
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    • 2015
  • ICP-AES has been used in many laboratories due to the advantages of wide calibration range and multi-element analysis, but it may give erroneous results and suffer from spectral interference due to the large number of emission lines associated with each element. In this study, certified reference materials (CRMs) and field samples were analyzed by ICP-AES and HG-AAS according to the official Korean testing method for soil pollution to investigate analytical problems. The applicability of HG-ICP-AES was also tested as an alternative method. HG-AAS showed good accuracies (90.8~106.3%) in all CRMs, while ICP-AES deviated from the desired range in CRMs with low arsenic and high Fe/Al. The accuracy in CRM030 was estimated as below 39% at the wavelength of 193.696 nm by ICP-AES. Significant partial overlaps and sloping background interferences were observed near to 193.696 nm with the presence of 50 mg/L Fe and Al. Most CRMs were quantified with few or no interferences of Fe and Al at 188.980 nm. ICP-AES properly assessed low and high level arsenic for field samples, at 188.980 nm and 193.696 nm, respectively. The importance of the choice of measurement wavelengths corresponding to relative arsenic level should be noted. Because interferences were affected by the sample matrix, operation conditions and instrument figures, the analysts were required to consider spectral interferences and compare the analytical performance of the recommended wavelengths. HG-ICP-AES was evaluated as a suitable alternative method for ICP-AES due to improvement of the detection limit, wide calibration ranges, and reduced spectral interferences by HG.

The Influence of Landscape Pavements on the WBGT of Outdoor Spaces without Ventilation or Shade at Summer Midday (조경포장이 옥외공간의 온열쾌적성지수(WBGT)에 미치는 영향 - 통풍과 차광이 배제된 하절기 주간의 조건에서 -)

  • Lee, Chun-Seok;Ryu, Nam-Hyung
    • Journal of the Korean Institute of Landscape Architecture
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    • v.38 no.2
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    • pp.1-8
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    • 2010
  • The purpose of the study was to evaluate the influence of landscaping pavements on WBGT(Wet-Bulb Globe Temperature) of outdoor spaces that lack ventilation and shade at summer midday. The relative humidity(RH), dry-bulb temperature(DT) and globe temperature(GT) were recorded every minute from June to October 2009 at a height of 1.2m above ten experimental beds with different pavements, by a measuring system consisting of an electric humidity sensor(GHM-15), resistance temperature detector(RTD, Pt-100), standard black globe(${\phi} 150mm$) and data acquisition systems(National Instrument's Labview and Compact FieldPoint). Additionally, the surface dry-bulb temperatures also were recorded and compared. The area of each experimental bed was 1.5m(W)${\times}$2.0m(L) and ten different kinds of pavement were used including grass, grass+cubic stone, grass+porous brick, brick, stone panels, cubic stone, interlocking blocks, clay brick, naked soil, gravel and concrete. To prevent interference from ventilation, a 1.5m height cubic steel frame was established around each bed and each vertical side of the frame was covered with transparent polyethylene film. Based on the records of the hottest period from noon to 3 PM on 26 days with a peak dry-bulb temperature over $30^{\circ}C$ at natural condition, the wet-bulb temperature(WT) and WBGT were calculated and compared. The major findings were as follows: 1. The average surface DT was $40.1^{\circ}C$, which is $9^{\circ}C$ higher than that of the natural condition. The surface DT of the pavements with grass were higher than those of concrete and interlocking block. The peak DT of the surface almost every pavement rose to above $50^{\circ}C$ during the hottest time. 2. The averages of DT, WT and GT were $40.1^{\circ}C$, $27.5^{\circ}C$ and $49.1^{\circ}C$, and the peak values rose to $48.1^{\circ}C$, $45.8^{\circ}C$ and $59.5^{\circ}C$, respectively. In spite of slight differences that resulted according to pavements, no coherent differentiating factor could be found. 3. The average WBGT of grass was the highest at $34.3^{\circ}C$ while the others were similar in the range of around $33{\pm}1^{\circ}C$. Meanwhile, the peak WBGT was highest with stone panel at $47.9^{\circ}C$. Though there were some differences according to pavements, and while grass seemed to be worst in terms of WBGT, it seems difficult to say ablolutely that grass was the worst because the measurement was conducted without ventilation and shade during summer daytime hours only, which had temperatures that rose to a dangerous degree(above $45^{\circ}C$ WBGT), withering the grass during the hottest period. The average WBGT resulted also showed that the thermal environment of the pavement without ventilation and shade were at an intolerable level for humans regardless of the pavement type. In summary, the results of this study show that ventilation and shade are more important factor than pavement type in terms of outdoor thermal comfort in summer daylight hours.

Development of Simultaneous Analytical Method for Determination of Isoxaflutole and its Metabolite (Diketonitrile) residues in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Isoxaflutole과 대사산물(Diketonitrile)의 동시시험법 개발)

  • Ko, Ah-Young;Kim, Heejung;Do, Jung Ah;Jang, Jin;Lee, Eun-Hyang;Ju, Yunji;Kim, Ji Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • The Korean Journal of Pesticide Science
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    • v.20 no.2
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    • pp.93-103
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    • 2016
  • A simultaneous analytical method was developed for the determination of isoxaflutole and metabolite (diketonitrile) in agricultural commodities. Samples were extracted with 0.1% acetic acid in water/acetonitrile (2/8, v/v) and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2 by 1 N hydrochloric acid. The analytes 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 ($0.02-2.0{\mu}g/mL$) for all the analytes into blank extract with $r^2$ > 0.997. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries were ranged between 72.9 to 107.3%, with relative standard deviations (RSDs) less than 10% for all analytes. All values were consistent with the criteria ranges requested in the Codex guideline (CAC/GL40, 2003). Furthermore, inter-laboratory study was conducted to validate the method. The proposed analytical method was accurate, effective, and sensitive for isoxaflutole and diketonitrile determination in agricultural commodities.

Development of Rapid Analytical Method of Forbidden Medicines in Dietary Supplements Using LC-ESI-Tandem MS (LC-ESI-tandem MS를 이용한 기능성표방식품 중 부정유해물질 신속검사체계 개발)

  • Kim, Hee-Yun;Jang, Young-Mi;Joo, Hyun-Jin;Jung, Young-Hyun;Lee, Myoung-Sook;Park, Jong-Seok;Lee, Kwang-Ho;Lee, Hwa-Mi
    • Korean Journal of Food Science and Technology
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    • v.39 no.4
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    • pp.372-379
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    • 2007
  • A high-performance liquid chromatography-electrospray ionization (HPLC-ESI) tandem MS was developed for the rapid and simultaneous determination of forbidden medicines in dietary supplements. Thirteen medicinal components such as PDE-5 inhibitors and their analogues, and the newly identified dimethylsildenafil and xanthoanthrafil, were included in this study. After tentative standardization of molecular ions in both polarities using thirteen references on the mass spectrometer, with ESI-continuous infusion via the syringe pump method, the relative intensity of the ions present in the resulting spectra was quantitatively compared. From the results, the ion mode was selected depending on each reference's characteristics. A HPLC method coupled with the ESI mode was developed considering the matrix effect and interference depending on the type of sample. The validation test of the developed method was followed by carrying out precision, accuracy, recovery, sensitivity and linearity, etc. The method showed sufficiently high sensitivity, reproducibility, and specificity, and produced 4 times faster results when compared with the existing HPLC/UV method for the determination of forbidden compounds in dietary supplements.

Development of an Official Analytical Method for Determination of Imazapyr in Agricultural Commodities using HPLC-UVD (HPLC-UVD를 이용한 농산물 중 Imazapyr의 공정분석법 확립)

  • Jang, Jin;Kim, Heejung;Ko, Ah-Young;Lee, Eun-Hyang;Joo, Yoon Ji;Kim, Jinhong;Chang, Moon-Ik;Rhee, Gyu-Seek
    • The Korean Journal of Pesticide Science
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    • v.19 no.1
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    • pp.5-13
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    • 2015
  • A chromatographic method for the determination of imazapyr, a non-selective herbicide, in agricultural commodities was developed to use safety control of pesticide residue on crops, and was fully validated as an official method for residue analysis. Agricultural commodities, mandarin (fruit), hulled rice (cereal grains), pepper (vegetables), potato (potatoes) and soybean (beans) were extracted with methanol and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2.5 by 4N hydrochloric acid. Finally, they were analyzed by high performance liquid chromatography coupled to UV detector (HPLC-UVD). The developed method had the linearity in the range of test concentrations with coefficients of determination ($r^2$) more than 0.99. Recovery studies were carried out at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. Recoveries were ranged between 72.1 to 108.0%, with relative standard deviations less than 10%. A consistent recovery was determined according to the CODEX guidelines (CAC/GL40, 2003). Finally, LC/MS with selected ion monitoring was also applied to confirm the suspected residues of imazapyr in agricultural samples. This developed method for determination of imazapyr residues in agricultural commodities. can be used as an official method.

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.

Location Environment and Vegetation Structure of the Aconitum austrokoreense Habitat (세뿔투구꽃 서식지의 입지환경 및 식생구조)

  • Cho, Seon-Hee;Lee, Kye-Han
    • Journal of Korean Society of Forest Science
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    • v.110 no.2
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    • pp.165-178
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    • 2021
  • Owing to the lack of consistent research on endangered plant species in Korea, there are insufficient data to preservespecies and expand habitats. This study analyzed the preferred habitat and threats to the survival of Aconitum austrokoreense, found on Baekwun Mountain in Gurye-gun, Gwangyang-si, Jeollanam-do Province, and classified as a level two endangered wild plant by the Ministry of Environment, by investigating major environmental factors such as climate, location, soil, and stand structure. By examining five selected sites inhabited by Aconitum austrokoreense on BaekwunMountain, this study found that the habitat had an altitude of 420 to 675 m above sea level and showed a northeast tendency, spreading over a range of inclination angles between 15° and 37°. The average number of plants across the five sites was 156. Site 4 (550 m) had the highest density of 372 plants, with an average height of 0.6 m. The average soil moisture and relative light intensity were 20.48% and 7.34%, respectively. Layer soil was presumed to be sandy loam, characterized by high sand content and good drainage. The habitat had average soil pH of 5.2, average organic matter of 16.46%, average nitrogen of 0.86%, average available phosphate of 11.86 mg/kg, average electrical conductivity of 0.44 dS/m, and average cation exchange capacity of 37.04 cmolc/kg. The total carbon in soil averaged 10.68%. From the analysis of the vegetation structure of sites inhabited by Aconitum austrokoreense, the dominant populations were Pinus koraiensis and Lindera erythrocarpa in Site 1, Magnolia obovata and Carpinus laxiflora in Site 2, Zelkova serrate and Quercus variabilis in Site 3, Staphylea bumalda and Lindera erythrocarpa in Site 4, and Morus bombycis,Styrax japonicus, and Carpinus laxiflora in Site 5. With most habitats located near trails and sap collection sites of Acer pictum, the species were exposed to artificial damage and interference threats.

Determination and Validation of an Analytical Method for Spiropidion and Its Metabolite Spiropidion-enol (SYN547305) in Agricultural Products with LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Spiropidion 및 대사산물 Spiropidion-enol (SYN547305) 시험법 개발 및 검증)

  • Gu, Sun Young;Lee, Su Jung;Shin, Hye-Sun;Kang, Sung Eun;Chung, Yun Mi;Lee, Jung Mi;Jung, Yong-hyun;Moon, Guiim
    • Korean Journal of Environmental Agriculture
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    • v.41 no.2
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    • pp.82-94
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    • 2022
  • BACKGROUND: Spiropidion and its metabolite are tetramic acid insecticide and require the establishment of an official analysis method for the safety management because they are newly registered in Korea. Therefore, this study was to determine the analysis method of residual spiropidion and its metabolite for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods (original, AOAC, and EN method) were applied to optimize the extraction method, and the EN method was finally selected by comparing the recovery test and matrix effect results. Various adsorbent agents were applied to establish the clean up method. As a result, the recovery of spiropidion was reduced when using the dispersive-SPE method with MgSO4, primary secondary amine (PSA), graphitized carbon black (GCB) and octadecyl (C18) in soybean. Color interference was minimized by selecting the case including GCB and C18 in addition to MgSO4. This method was established as the final analysis method. LC-MS/MS was used for the analysis by considering the selectivity and sensitivity of the target pesticide and the analysis was performed in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 79.4-108.4%, with relative standard deviation and coefficient of variation were less than 7.2% and 14.4%, respectively. CONCLUSION(S): Spiropidion and its metabolite could be analyzed with a modified QuEChERS method, and the established method would be widely available to ensure the safety of residual insecticides in Korea.

Abundance and Occupancy of Forest Mammals at Mijiang Area in the Lower Tumen River (두만강 하류 밀강 지역의 산림성 포유류 풍부도와 점유율)

  • Hai-Long Li;Chang-Yong Choi
    • Korean Journal of Environment and Ecology
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    • v.37 no.6
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    • pp.429-438
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    • 2023
  • The forest in the lower Tumen River serves as an important ecosystem spanning the territories of North Korea, Russia, and China, and it provides habitat and movement corridors for diverse mammals, including the endangered Amur tiger (Panthera tigris) and Amur leopard (Panthera pardus). This study focuses on the Mijiang area, situated as a potential ecological corridor connecting North Korea and China in the lower Tumen River, playing a crucial role in conserving and restoring the biodiversity of the Korean Peninsula. This study aimed to identify mammal species and estimate their relative abundance, occupancy, and distribution based on the 48 camera traps installed in the Mijiang area from May 2019 to May 2021. The results confirmed the presence of 18 mammal species in the Mijiang area, including large carnivores like tigers and leopards. Among the dominant mammals, four species of ungulates showed high occupancy and detection rates, particularly the Roe deer (Capreolus pygargus) and Wild boar (Sus scrofa). The roe deer was distributed across all areas with a predicted high occupancy rate of 0.97, influenced by altitude, urban residential areas, and patch density. Wild boars showed a predicted occupancy rate of 0.73 and were distributed throughout the entire area, with factors such as wetland ratio, grazing intensity, and spatial heterogeneity in aspects of the landscape influencing their occupancy and detection rates. Sika deer (Cervus nippon) exhibited a predicted occupancy rate of 0.48, confined to specific areas, influenced by slope, habitat fragmentation diversity affecting detection rates, and the ratio of open forests impacting occupancy. Water deer (Hydropotes inermis) displayed a very low occupancy rate of 0.06 along the Tumen River Basin, with higher occupancy in lower altitude areas and increased detection in locations with high spatial heterogeneity in aspects. This study confirmed that the Mijiang area serves as a habitat supporting diverse mammals in the lower Tumen River while also playing a crucial role in facilitating animal movement and habitat connectivity. Additionally, the occupancy prediction model developed in this study is expected to contribute to predicting mammal distribution within the disrupted Tumen River basin due to human interference and identifying and protecting potential ecological corridors in this transboundary region.