• Title/Summary/Keyword: method detection limit

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Study on Improvement in Reliability of Measurement and Analysis for Polycyclic Aromatic Hydrocarbons in the Atmosphere (대기 중 다환방향족탄화수소(PAHs)의 측정.분석 신뢰도 향상에 관한 고찰)

  • Lee, Min-Do;Lim, Yong-Jae;Lee, Sang-Uk;Kong, Boo-Joo;Lee, Sang-Deok;Han, Jin-Seok
    • Journal of Korean Society for Atmospheric Environment
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    • v.23 no.5
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    • pp.515-525
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    • 2007
  • In this study, various techniques for measurement and analysis of PAHs in the ambient air were verified in order to select a more reliable method. Sampling and analysis of PAHs were done by the EPA TO-13a method. QA/QC of the measurement was conducted to minimize errors in sampling and analyzing processes. The linearity of calibration curve of the PAH standards was good ($R^2{\geq}0.99$). Audit accuracy was evaluated using 5 internal standards of PAHs ($Naphthalene-d_8,\;Acenaphthene-d_{10},\;Phenanthrene-d_{10},\;Chrysene-d_{12},\;Perylene-d_{12}$). Relative standard deviations of the internal standard of the PAHs were ranged from 6.22% for $acenaphthene-d_{10}$ to 8.11% for $chrysene-d_{12}$. To evaluate the surrogate recoveries, two field surrogate standards of PAHs ($fluoranthene-d_{10},\;benzo(a)pyrene-d_{12}$) and two extract surrogate standards of the PAHs ($fluorene-d_{10},\;pyrene-d_{12}$) were spiked into all samples before field sampling and sample extraction, respectively. Recoveries of field the surrogate standards ranged from $80.4{\pm}12.2%$ for $fluoranthene-d_{10}$ to $66.2{\pm}12.8%$ for $benzo(a)pyrene-d_{12}$. Extraction recoveries of the surrogate standards ranged from $70.4{\pm}10.2%$ for $fluorene-d_{10}$ to $77.6{\pm}10.8%$ for $pyrene-d_{10}$. The detection limit of benzo(a)pyrene among 16 PAHs standards for quantitation was 20 pg.

Application of Freezing Filtration Method to the Analysis of Alkylphenols, Chlorophenols and Bisphenol a in Korean Aquatic Biological Samples Using GC/MS-SIM (GC/MS-SIM을 이용한 우리나라 수중 생물시료 중 알킬페놀, 클로로페놀과 비스페놀 A의 분석을 위한 냉동필터법의 응용)

  • Kim, Hyub;Jang, Cheol-Hyeon
    • Journal of Korean Society of Environmental Engineers
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    • v.29 no.6
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    • pp.689-698
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    • 2007
  • A new technique was proposed for the determination of alkylphenols, chlorophenols and bisphenol A in korean aquatic biological samples. The alkylphenols, chlorophenols and bisphenol A in korean aquatic biological samples were extracted with acetonitrile and then acetonitrile layer was refrigerated at $-60^{\circ}C$ for 2 hours(freezing filtration method). Also, solid-phase extraction(SPE) was used to XAD-4 and subsequent conversion to isobutoxycarbonyl(isoBOC) or tert-butyldimethylsilyl(TBDMS) derivatives for sensitive analysis with gas chromatography/mass spectrometry-selected ion monitoring(GC/MS-SIM) mode. For isoBOC derivatization and TBDMS derivatization the recoveries were $70.1\sim150.6%$ and $93.8\sim108.3%$, the method detection limit(MDLs) of bisphenol A for SIM were $0.062{\mu}g/kg$ and $0.010{\mu}g/kg$, and the SIM respectively. When these methods were applied to korean aquatic biological samples, the concentrations of the 11 phenolic EDCs were $0.675\sim1.970{\mu}g/kg$.

An analytical method of soap biodegradability with fatty acid p-BPB derivatives (지방산의 p-BPB 유도체에 의한 비누 생분해도 분석 방법)

  • Oh, Se-Woong;Lee, Ja-Kyoung;Chung, Yong;Chang, Sug-Youn;Kim, Yeo-Kyung
    • Analytical Science and Technology
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    • v.6 no.1
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    • pp.9-19
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    • 1993
  • Fatty acid salts derived from soap can be transferred into a typical derivative with p-bromophenacyl bromide using crown ether, a catalizer by the solid-liquid phase transfer reaction in nonpolar, aprotic solvents and separated by the reverse phase high performance liquid Chromatography (RP-HPLC) and determined using UV detector. The minimal limit of detection was defined at approximately 10~50ng in accordance with the chain length. The derivatization reaction in the presence of EDTA can be applied mot only to the calcium salts but also to the other various metal salts. The recoveries of fatty acid derivatizations in the absence and presence of the midium containing the yeast extract were obtained $95.4{\pm}1.2$, and $85.2{\pm}2.4%$ respectively. The analytical method would be applicable to determine the biodegradation of fatty acid salts in nature as well as in artificial condition such as shaker flask-medium method.

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Determination of Neonicotinoid Pesticides in Commercial Agricultural Products by LC-MS/MS (LC-MS/MS를 이용한 농산물중 Neonicotinoid 계 농약분석)

  • Hwang, Lae-hong;Yang, Hye-ran;Lee, Jae-kyoo;Kim, Chang-kyu;Kim, Min-jung
    • Journal of Food Hygiene and Safety
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    • v.35 no.4
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    • pp.312-318
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    • 2020
  • A method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for neonicotinoid pesticide analysis in agricultural products. Four compounds (imidacloprid, clothianidin, acetamiprid, thiacloprid) were extracted with acetonitrile from agricultural products and cleaned up by NH2 solid-phase extraction procedure, and eluted with 0.1% formic acid in methanol/dichloromethane (5/95, v/v). The limit of detection and quantification were 0.0001-0.0005 mg/kg and 0.001 mg/kg, respectively. The mean recoveries of neonicotinoid pesticide from agricultural products were in the range of 90.7-100.9% and 94.4-99.8%, as spiked at 0.2 mg/kg and 0.02 mg/kg, respectively. This validation satisfied the national criteria for pesticide analytical methods. In summary, The present method is fast, precise and sensitive enough for the Positive List System (PLS), and we conclude that the method is also suitable for neonicotinoid pesticide determination in a wide range of agricultural products.

Determination of Niacin in Infant Formula by Solid-phase Clean-up and HPLC with Photodiode Array Detector (고체상 정제 및 HPLC/PDA에 의한 영유아식 중 나이아신의 분석)

  • Hong, Jee-Eun;Kim, Mi-Ran;Cheon, Sang-Hee;Chai, Jung-Young;Park, Eun-Ryong;Mun, Chun-Sun;Gwak, In-Shin;Kim, Ok-Hee;Lee, Kwang-Ho
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.38 no.3
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    • pp.359-363
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    • 2009
  • This study was performed to establish a rapid and simple analytical method for niacin (nicotinic acid and nicotinamide) using HPLC. A pretreatment method for the extraction and clean-up of niacin in infant formula sample and an instrumental condition for HPLC were optimized. Niacin was extracted by 5 mM hexanesulfonate with ultrasonication for 30 min. For the clean-up of the sample, the extract was applied to a HLB cartridge, and then niacin was eluted from the cartridge using 5 mL of 80% methanol after washing with 5 mL of n-hexane. The total recoveries were $83{\sim}104%$ and relative standard deviation were in the range of $1.5{\sim}3.5%$ during the extraction and clean-up process. Niacin was determined by gradient elution with sodium hexanesulfonate/methanol buffer as a mobile phase and a photodiode array detector (260 nm). It showed a high linearity between the content of niacin and the peak area ($r^2$=1.000) in the range of $0.02{\sim}10.0$ mg/L of nicotinic acid and nicotinamide. The detection limit was 0.02 mg/L (0.2 mg/kg in the sample). The method was successfully applied for the determination of niacin in infant formula. Total niacin contents were in the range of $53.5{\sim}140.3$ mg/kg.

Development of an Official Method for Measurement of Fluazinam Residues for Quarantine of Imported and Exported Horticultural Products (수출입 원예작물의 검역을 위한 살균제 Fluazinam의 공정 잔류분석법 개발)

  • Kim, Gyeong-Ha;Ahn, Kyung-Geun;Kim, Gi-Ppeum;Hwang, Young-Sun;Chang, Moon-Ik;Kang, In-Kyu;Lee, Young Deuk;Choung, Myoung-Gun
    • Horticultural Science & Technology
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    • v.34 no.1
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    • pp.183-194
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    • 2016
  • This experiment was conducted to establish an official determination method to measure fluazinam residue in horticultural crops for import and export using GC-ECD/MS. Fluazinam residue was extracted with acetone from fresh samples of four representative horticultural products, the vegetable crops green pepper and kimchi cabbage, and the fruit crops mandarin and apple. The acetone extract was diluted with saline water and n -hexane partitioning was used to recover fluazinam from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fluazinam was separated and quantitated by GC with ECD using a DB-17 capillary column. The horticultural crops were fortified with three different concentrations of fluazinam. Mean recoveries ranged from 82.5% to 99.9% in the four crops. The coefficients of variation were less than 10.0%. The quantitative limit of fluazinam detection was $0.004mg{\cdot}kg^{-1}$ in the four crop samples. GC/MS with selected-ion monitoring was also used to confirm the suspected residue. This analytical method was reproducible and sensitive enough to measure the residue of fluazinam in horticultural commodities for import and export.

Determination of mandipropamid residues in agricultural commodities using high-performance liquid chromatography with mass spectrometry (고성능액체크로마토그래피를 이용한 농산물 중 Mandipropamid의 잔류분석법 확립)

  • Kwon, Chan Hyeok;Chang, Moon Ik;Im, Moo Hyeog;Choi, Hoon;Jung, Da I;Lee, Su Chan;Yu, Jin Young;Lee, Young Deuk;Lee, Jong Ok;Hong, Moo Ki
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.518-525
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    • 2008
  • Mandipropamid is a new mandelamide-type fungicide to control foliar Oomycete pathogens in some vegetables. An analytical method was developed to determine mandipropamid residues in agricultural commodities using high-performance liquid chromatography (HPLC) and liquid chromatography/mass spectrometry (LC/MS). Mandipropamid was extracted with methanol from grape, tomato, green pepper, Chinese cabbage and potato samples. The extract was diluted with saturated sodium chloride solution and distilled water, and dichloromethane partition was followed to recover the mandipropamid from the aqueous phase. Florisil column chromatography was employed to further remove interfering co-extractives prior to HPLC analysis. Reverse-phased HPLC was successfully applied to determine mandipropamid in sample extracts with the detection at its ${\lambda}_{max}$ (223 nm). Overall recoveries of mandipropamid from fortified samples averaged $99.8{\pm}1.7$ (n=6), $89.3{\pm}5.3$ (n=6), $98.7{\pm}2.2$ (n=6), $99.7{\pm}6.8$ (n=6) and $91.1{\pm}3.1$ (n=6) for grape, tomato, green pepper, Chinese cabbage and potato, respectively. Limit of quantification of the method was 0.02~0.04 mg/kg for all samples. A LC/mass spectrometry with selected-ion monitoring was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to determine the terminal residue of mandipropamid in agricultural commodities.

Introduction of a New Method for Total Organic Carbon and Total Nitrogen Stable Isotope Analysis of Dissolved Organic Matter in Aquatic Environments (수환경 내 용존성 유기물질의 총 유기탄소 및 총 질소 안정동위원소 신규 분석법 소개)

  • Si-yeong Park;Heeju Choi;Seoyeon Hong;Bo Ra Lim;Seoyeong Choi;Eun-Mi Kim;Yujeong Huh;Soohyung Lee;Min-Seob Kim
    • Korean Journal of Ecology and Environment
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    • v.56 no.4
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    • pp.339-347
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    • 2023
  • Dissolved organic matter (DOM) is a key component in the biogeochemical cycling in freshwater ecosystem. However, it has been rarely explored, particularly complex river watershed dominated by natural and anthropogenic sources, such as various effluent facility and livestock. The current research developed a new analytical method for TOC/TN (Total Organic Carbon/Total Nitrogen) stable isotope ratio, and distinguish DOM source using stable isotope value (δ13C-DOC) and spectroscopic indices (fluorescence index [FI] and biological index [BIX]). The TOC/TN-IR/MS analytical system was optimized and precision and accuracy were secured using two international standards (IAEA-600 Caffein, IAEA-CH-6 Sucrose). As a result of controlling the instrumental conditions to enable TOC stable isotope analysis even in low-concentration environmental samples (<1 mgC L-1), the minimum detection limit was improved. The 12 potential DOM source were collected from watershed, which includes top-soils, groundwater, plant group (fallen leaves, riparian plants, suspended algae) and effluent group (pig and cow livestock, agricultural land, urban, industry facility, swine facility and wastewater treatment facilities). As a result of comparing characteristics between 12 sources using spectroscopic indices and δ13C-DOC values, it were divided into four groups according to their characteristics as a respective DOM sources. The current study established the TOC/TN stable isotope analyses system for the first time in Korea, and found that spectroscopic indices and δ13C-DOC are very useful tool to trace the origin of organic matter in the aquatic environments through library database.

Soil Residues and Absorption-translocation into Red Lettuce and Young Radish Crops of Veterinary Antibiotics According to Agricultural Water Irrigation Method (농업용수 관개방법에 따른 축산용 항생제의 토양중 잔류와 적상추와 열무 작물로의 흡수·이행)

  • Park, Young-Jae;Jeon, Hee-Su;Cho, Jae-Young
    • Korean Journal of Organic Agriculture
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    • v.32 no.1
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    • pp.107-125
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    • 2024
  • Three types of veterinary antibiotics, including oxytetracycline (OTC) and chlortetracycline (CTC) of tetracycline class and amoxicillin (AMX) of penicilline class, were artificially introduced into the irrigation water. The residue of veterinary antibiotics in the soil, the absorption-translocation of veterinary antibiotics into the red lettuce and young radish plant, and crops yield were investigated according to the agricultural water irrigation method (surface drip irrigation, underground drip irrigation, and sprinkler irrigation). There was no significant difference in the residue and translocation of veterinary antibiotics in the soils and crops according to the irrigation method and type of veterinary antibiotics (p>0.05). For the edible parts of red lettuce and young radish, all three types of veterinary antibiotics were found to be below the detection limit, indicating that the safety of the crops was secured. The translocation factor of red lettuce and young radish were found to be less than 0.3 and 0.2, respectively. However, continuous introduction of veterinary antibiotics in agricultural arable lands may have negative effects by affecting soil microbial activity and soil microbe species diversity, so continuous management is deemed necessary.

A Study on Multi-Object Data Split Technique for Deep Learning Model Efficiency (딥러닝 효율화를 위한 다중 객체 데이터 분할 학습 기법)

  • Jong-Ho Na;Jun-Ho Gong;Hyu-Soung Shin;Il-Dong Yun
    • Tunnel and Underground Space
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    • v.34 no.3
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    • pp.218-230
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    • 2024
  • Recently, many studies have been conducted for safety management in construction sites by incorporating computer vision. Anchor box parameters are used in state-of-the-art deep learning-based object detection and segmentation, and the optimized parameters are critical in the training process to ensure consistent accuracy. Those parameters are generally tuned by fixing the shape and size by the user's heuristic method, and a single parameter controls the training rate in the model. However, the anchor box parameters are sensitive depending on the type of object and the size of the object, and as the number of training data increases. There is a limit to reflecting all the characteristics of the training data with a single parameter. Therefore, this paper suggests a method of applying multiple parameters optimized through data split to solve the above-mentioned problem. Criteria for efficiently segmenting integrated training data according to object size, number of objects, and shape of objects were established, and the effectiveness of the proposed data split method was verified through a comparative study of conventional scheme and proposed methods.