• Title/Summary/Keyword: method detection limit

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Determination of Trichlorfon Pesticide Residues in Milk via Gas Chromatography with μ-Electron Capture Detection and GC-MS

  • Hem, Lina;Khay, Sathya;Choi, Jeong-Heui;Morgan, E.D.;El-Aty, A.M. Abd;Shim, Jae-Han
    • Toxicological Research
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    • v.26 no.2
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    • pp.149-155
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    • 2010
  • The pesticide trichlorfon is readily degraded under experimental conditions to dichlorvos. A method has therefore been developed by which residues of trichlorfon in milk are determined as dichlorvos, using gas chromatography with ${\mu}$-electron capture detection. The identification of dichlorvos was confirmed by mass spectrometry. Milk was extracted with acetonitrile followed by centrifugation, freezing lipid filtration, and partitioning into dichloromethane. The residue after partitioning of dichloromethane was dissolved in ethyl acetate for gas chromatography. Recovery concentration was determined at 0.5, 1.0, and 2.0 of times the maximum permitted residue limits (MRLs) for trichlorfon in milk. The average recoveries (n = 6) ranged from 92.4 to 103.6%. The repeatability of the measurements was expressed as relative standard deviations (RSDs) ranging from 3.6%, to 6.7%. Limit of detection (LOD) and limit of quantification (LOQ) were 3.7 and $11.1{\mu}g/l$, respectively. The accuracy and precision (expressed as RSD) were estimated at concentrations from 25 to $250{\mu}g/l$. The intra- and inter-day accuracy (n = 6) ranged from 89.2% to 91% and 91.3% to 96.3%, respectively. The intra- and inter-day precisions were lower than 8%. The developed method was applied to determine trichlorfon in real samples collected from the seven major cities in the Republic of Korea. No residual trichlorfon was detected in any samples.

An Enzyme-Linked Immunosorbent Assay for Detection of Pantothenic Acid (판토텐산의 분석을 위한 효소면역측정법)

  • Shon, Dong-Hwa;Park, Youn-Sick;Bae, Gun-Won
    • Korean Journal of Food Science and Technology
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    • v.32 no.5
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    • pp.1009-1014
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    • 2000
  • In order to detect pantothenic acid (PA), conditions for enzyme-linked immunosorbent assay (ELISA) were established. Anti-PA-BSA antibody was produced from rabbits immunized with PA-bovine serum albumin (BSA) conjugates which were prepared by the bromoacetyl chloride [Bc] method (PA-BSA[Bc]) and by the periodate oxidation [Po] method (PA-BSA[Po]). PA-BSA[Bc] and PA-BSA[Po] was used as a coating antigen for competitive indirect(ci)ELISA. The Anti-PA-BSA[Po] antibody on ciELISA showed no competitive reaction. The detection limit of PA by ciELISA using Anti-PA-BSA[Bc] antibody was 1 ppm. The Anti-PA-BSA[Bc] antibody showed little cross-reactivity to PA derivatives such as pantoyllactone, pantetheine, pantothenyl alcohol, and acetyl CoA. The detection limit of PA by microbiological assay (MBA) was 10 ppb. Assay recoveries of PA in egg, cow's liver, and lettuce by ciELISA were 109, 64, and 344%, respectively, comparing with the MBA results.

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Determination of cyromazine in commercial insecticides using HPLC-DAD

  • Kim, Young-Wook;Han, Bok Hee;Kang, Young Eun;Rhee, Chae Hong;Seo, Sang-Ji;Kim, Soohee;Jeong, Wooseog;Her, Moon
    • Korean Journal of Veterinary Service
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    • v.43 no.4
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    • pp.261-265
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    • 2020
  • Each commercial cyromazine insecticide has different HPLC conditions. The aim of this study was to establish a standardized chromatographic method for the determination of cyromazine in commercial insecticides. The separation was achieved on two C18 columns - Waters® Bondapak C (4×300 nm i.d., 10 ㎛) and X bridge (4.6×250 nm i.d., 5 ㎛) using a mobile phase composed of water/methanol/ethanolamine (76:24:0.1, v/v), with UV detection at wavelengths 230 nm and 254 nm. A total of six commercial cyromazine insecticides were analyzed. In this study, the optimal high-performance liquid chromatography conditions for the analysis of cyromazine were as follows: a mobile phase of water/methanol/ethanolamine (76:24:0.1, v/v) at a flow rate of 1.0 mL/min and a detection wavelength of 230 nm using a X bridge C18 column (4.6×250 nm i.d., 5 ㎛) at a column temperature of 25℃. The calibration curve was linear in the concentration range of 5~50 ㎍/mL, with a correlation coefficient of 0.99995. The cyromazine detection limit was 0.2 ㎍/mL, and the limit of quantification was 0.59 ㎍/mL. The percentage recovery ranged from 99.8% to 101.0% for cyromazine, and the relative standard deviation was not over 2.0%. The cyromazine concentration ranged from 92.7% to 109.4% and was within the acceptable range (90~120%) for the percent of the labeled amount. This method was found to be suitable for determining cyromazine in commercial insecticides.

Method validation for quantitative analyzing aflatoxin productivity in Aspergillus sp. isolated from soybean paste

  • SeongEui Yoo;WooSoo Jeong;Soo-Hwan Yeo;So-Young Kim
    • Food Science and Preservation
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    • v.30 no.1
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    • pp.28-41
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    • 2023
  • Non-aflatoxigenic Aspergillus oryzae and aflatoxigenic A. flavus cannot be clearly identified by partial sequencing of the internal transcribed spacer (ITS) and 18S ribosomal ribonucleic acid (18S rRNA) regions. This study aimed to compare the accuracy among three aflatoxin detection methods using ultra-performance liquid chromatography (UPLC), high-performance liquid chromatography (HPLC), and an enzyme-linked immunosorbent assay (ELISA) kit and to select the non-aflatoxigenic Aspergillus sp. isolated from soybean paste. All analytical methods were suitable according to the international standards of Codex Alimentarius FAO-WHO (CODEX) or the Ministry of Food and Drug Safety (MFDS). UPLC exhibited the best of limit of detection (LOD) and limit of quantification (LOQ). Based on UPLC, HPLC, and the ELISA kit assay, the P5 and P7 strains isolated from soybean paste had 1,663.49, 1,468.12, and >20 ㎍/kg and 1,470.08, 1,056.73, and >20 ㎍/kg, respectively, detected and re-identified as A. flavus. In contrast, the P3 and P4 strains (A. oryzae), which were detected below the MFDS standards in all assays, were confirmed as non-aflatoxigenic fungi. Among the methods evaluated for quantitative analysis of aflatoxin, UPLC and HPLC are superior in terms of accuracy, and the ELISA kit rapidly detects low concentrations of aflatoxin. Furthermore, this study demonstrates that any Aspergillus sp. isolated for use as a fermentation starter should be analyzed for potential aflatoxin production using UPLC and HPLC for accurate quantitative analysis or ELISA for the rapid detection of low-level concentrations of aflatoxin.

Analysis of Butyltin Compounds(mono-, di-, and tributyltin) in Human Blood (혈액 중의 주석화합물(MBT, DBT, TBT)의 분석과 농도에 관한 연구)

  • Kim, Nam Sook;Park, Dong Uk;Oh, Jae Ryoung;Shim, Woon Joon
    • Analytical Science and Technology
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    • v.14 no.2
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    • pp.115-122
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    • 2001
  • Butyltin compounds, including mono-(MBT), di-(DBT) and tributyltin(TBT) were analyzed in 44 human blood samples randomly collected from a hospital in "K" a city. Gas chromatograph equipped with flame photometric detector(FPD) was used to quantify the amounts of butylin compounds. Method detection limits(MDL) of this analytical method were 3.69ng Sn/g for MBT, 0.91ng Sn/g for DBT and 1.09ng Sn/g wet wt for TBT respectively. Standard reference material(SRM) containing of $1.3{\mu}g/g$ TBT as chloride was analyzed to check if this analytical results would be reliable. Recovery of about 90% was obtained through this analysis, indicating that the analytical method from butyltin compounds blood was reliable. The concentrations of butyltin compounds ranged MDL(<3.69) to 7.93ng Sn/g for MBT and 1.15 to 5.41ng Sn/g wet wt for DBT. Tributyltin was below detection limit in all samples. Detection limits of our results are lower than those reported by Kannan et al. who reported butyltin compounds in 33 human blood samples in the United States. Detection of MBT and DBT on blood sample implies that butyltin compounds could be absorbed through consumption of seafoods or exposure to food stuffs made of plastics and household items. Further study is needed to examine if butyltin compounds in blood can be reliably analyzed and used as intake index.

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A Study on the Analysis of Polycyclic Aromatic Hydrocarbons by RPLC/DAD (I) (RPLC/DAD를 이용한 Polycyclic Aromatic Hydrocarbon류의 분석에 관한 연구(I))

  • Lee, Won;Hong, Jee-Eun;Park, Song-Ja;Pyo, Hee Soo
    • Analytical Science and Technology
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    • v.10 no.5
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    • pp.315-324
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    • 1997
  • The retention behaviors of 16 PAHs and 4 nitro-PAHs were studied with several parameters involved numbers of carbon atoms, F factor, aqueous solubility, L/B ratio, and numbers of interfering hydrogen atom pairs on the chemical structures of PAHs by using reversed-phase liquid chromatography/diode array detection method (RPLC/DAD) and gradient elution method. It was obtain that the log k' for most of PAHs with increasing the number of carbon and the F factor in their molecules. Chromatographic retention of PAH isomers and nitro-PAHs were examined with aqueous solubility, L/B ratio and number of interfering hydrogen atom pairs. As a result of comparison with these factors and retention times, it was found that those solutes having larger aqueous solubilities and greater L/B ratios were retained longer on stationary phase. This tendency was also occured in the molecules having the more number of interfering hydrogen atom pairs. Detection limits of PAHs which were obtained with three times measurements by RPLC/DAD were in the range of 100~500ng/mL and method detection limit(MDL) for water sample were in the range of 0.1~0.5ng/mL.

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Ship Detection from Satellite Radar Imagery using Stepwise Threshold Determination (단계적 임계치 결정을 통한 위성레이더이미지 내 선박 탐지)

  • Ho-Kun Jeon;Hong Yeon Cho
    • Proceedings of the Korean Institute of Navigation and Port Research Conference
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    • 2023.05a
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    • pp.152-153
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    • 2023
  • AIS has been widely used for maritime traffic assessment for its convenience. However, AIS has problems with position missing due to radio interference and transmission distance limit. On the other hand, satellite radar determines the location of ships over a wide sea regardless of the problems. This study proposes a noble method of stepwise threshold determination to detect ships from Sentinel-1. The proposed method is up to 25 times faster than the existing moving window-based threshold determination method, and the detection accuracy is similar.

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A Study on Occupational Environment Assessment Strategies for Respirable Particulate Matter at Coal-Fired Power Plants (석탄화력발전소 호흡성분진 작업환경 평가 전략 사례에 관한 연구)

  • Eun-Seung Lee;Yun-Keun Lee;Dong-Il Shin
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.33 no.3
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    • pp.375-383
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    • 2023
  • Objectives: Coal-fired power plants feature diverse working conditions, including multi-layered employment structures and irregular work cycles due to outsourcing and non-standardized tasks. The current uniform occupational environment measurement systems have limitations in accurately assessing and evaluating these varied conditions. This study aims to propose alternative measurement and assessment strategies to supplement existing methods. Methods: Major domestic coal-fired power plants were selected as the study targets. To prepare for the study and establish strategies, work processes were identified and existing occupational environment measurement results were compared and analyzed. The study proceeded by employing three strategies: specific exposure groups (SEGs) measurement, continuous monitoring, and supplementary measurements, which were then compared and discussed. Results: Previous exposure index evaluations (5,268 cases) indicated that crystalline silica, a type of respirable particulate matter, had detection limits below the threshold (non-detectable) in 82.6% (4,349 cases) of instances. Exposures below 10% of the exposure limit were observed at a very low concentration of 96.1%. Similar exposure group measurements yielded results where detection limits were below the threshold in 38.2% of cases, and exposures below 10% of the limit were observed in 70.6%. Continuous monitoring indicated detection limits below the threshold in 12.6% of cases, and exposures below 10% of the limit were observed in 75.6%. Instances requiring active workplace management accounted for more than 30% of cases, with SEGs at 11.8% (four cases), showing a higher proportion compared to 3.0% (four cases) in continuous monitoring. For coal dust, exposures below 10% of the limit were highest in legal measurements at 90.2% (113 cases), followed by 74.0% (91 cases) in continuous monitoring, and 47.0% (16 cases) in SEGs. Instances exceeding 30% were most prevalent in SEGs at 14.7% (five cases), followed by legal measurements at 5.0% (eight cases), and continuous monitoring at 2.4% (three cases). When examining exposure levels through arithmetic means, crystalline silica was found to be 104.7% higher in SEGs at 0.0088 mg/m3 compared to 0.0043 mg/m3 in continuous monitoring. Coal dust measurements were highest in SEGs at 0.1247 mg/m3, followed by 0.1224 mg/m3 in legal measurements, and 0.0935 mg/m3 in continuous monitoring. Conclusions: Strategies involving SEGs measurement and continuous monitoring can enhance measurement reliability in environments with irregular work processes and frequent fluctuations in working conditions, as observed in coal-fired power plants. These strategies reduce the likelihood of omitting or underestimating processes and enhance measurement accuracy. In particular, a significant reduction in detection limits below the threshold for crystalline silica was observed. Supplementary measurements can identify worker exposure characteristics, uncover potential risks in blind spots of management, and provide a complementary method for legal measurements.

Comparison of IHNV Detection Limits by IMS-RT-PCR, Western Blot and ELISA

  • Kim Soo-Jin;Lee Eun-Young;Oh Myung-Joo;Choi Tae-Jin
    • Fisheries and Aquatic Sciences
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    • v.4 no.1
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    • pp.32-38
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    • 2001
  • Several molecular biological techniques have been used to detect virus rapidly and accurately, but these methods have limitations in the early stage of viral infection with very low concentration of virus. We compared the detection limits of IMS-PCR, Western blot and ELISA with infectious hematopoietic necrosis virus OHNV). Four antibodies, rabbit anti-IHNV polyclonal antibody, anti-IHNV nucleocapsid protein monoclonal antibody, anti-IHNV nucleocapsid protein polyclonal antibody, and anti-IHNV glycoprotein polyclonal antibody, were tested to find out the most effective antibody for each method. The detection limit with IMS- PCR was $2\times10^6$ pfu when the viral RNA was extracted before RT-PCR. In the western blot with rabbit anti­IHNV polyclonal antibody one pfu of virus could be detected. In ELISA, 10 pfu of virus particles were detected with the same antibody.

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Ultra-sensitive Determination of Salinomycin in Serum Using ICP-MS with Nanoparticles

  • Cho, H.K.;Lim, H.B.
    • Bulletin of the Korean Chemical Society
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    • v.35 no.11
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    • pp.3195-3198
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    • 2014
  • An ultra-sensitive detection method for small molecules such as antibiotics was developed using ICP-MS with magnetic and $TiO_2$ nanoparticles. Since most of the antibiotics are too small to employ a sandwich-type extraction through an immunoreaction, a non-specific platform was employed, in which the target was extracted by magnetic separation, followed by tagging with $TiO_2$ nanoparticles of 11.2 nm for ICP-MS measurement. The detection limit for salinomycin obtained from spiked serum samples was $0.4ag\;mL^{-1}$ (${\pm}10.3%$), which was about $1.5{\times}10^6$ times lower than that of LC-MS/MS and about $1.2{\times}10^{11}$ times better than that of ELISA. Such an excellent sensitivity enabled us to study the toxicity of antibiotics exposed to human beings by determining them in serum.