• Title/Summary/Keyword: limit of detection

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Development of Simultaneous Analytical Method of Veterinary Antibiotics in Manure using Liquid Chromatography Coupled with Tandem Mass Spectrometry (LC-MS/MS를 이용한 퇴비 및 액비 중 항생제 동시 분석법 개발)

  • Chung, Hyung Suk;Lee, Young Jun;Lee, Han Sol;Rahman, Md. Musfiqur;Kabir, Md. Humayun;Park, Byung-Jun;Kim, Jang-Eok;Shim, Jae-Han
    • Korean Journal of Environmental Agriculture
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    • v.36 no.3
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    • pp.201-210
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    • 2017
  • BACKGROUND: The current study was to monitor of 9 veterinary antibiotics (ceftiofur, clopidol, florfenicol, sulfamethazine, sulfamethoxazole, sulfathiazole, tetracycline, tiamulin, and tylosin) in manure using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive and negative electrospray ionization mode. METHODS AND RESULTS: Sample preparation was carried out using Mcllvaine buffer and citrate salts to adjust the pH of the sample followed by purification with dispersive solid phase extraction (d-SPE). Separation of analytes during LC-MS/MS analysis was conducted using an Eclipse Plus $C_{18}$ column and the mobile phase was in gradient mode with, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations of all tested antibiotics was good, with $R^2$ determination coefficients ${\geq}0.9920$. The limit of detection (LOD) and quantifications (LOQ) were $0.1-67.0{\mu}g/kg$ and $0.4-200.0{\mu}g/kg$, respectively. Analysis of 13 solid and liquid manure samples taken from the Republic of Korea revealed concentrations less than $0.7{\mu}g/kg$ for tiamulin, $1497.6{\mu}g/kg$ for sulfamethazine. CONCLUSION: To monitor 9 veterinary antibiotics from manure samples in 13 provincial areas throughout the Republic of Korea, an analytical method was developed. The developed method was fully validated and successfully applied for monitoring various veterinary antibiotics in manure samples.

A Study on the Efficient Measurement of Airborne Asbestos Concentrations at Demolition Sites of Asbestos Containing Buildings, etc. in Seoul (서울시내 석면함유 건축물 철거 현장 등에서의 효과적인 공기 중 석면농도 측정을 위한 연구)

  • Lee, Jinhyo;Lee, Suhyun;Kim, Jeongyeun;Kim, Jihui;Chung, Sooknye;Kim, Jina;Oh, Seokryul;Kim, Iksoo;Shin, Jinho;Eo, Soomi;Jung, Kweon;Lee, Jinsook
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.24 no.2
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    • pp.113-121
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    • 2014
  • Objectives: This study is intended to seek credible and efficient measurements on airborne asbestos concentrations that allow immediate action by establishing complementary data through comparative analysis with existing PCM and KF-100 method real-time monitoring equipment in working areas in Seoul where asbestos-containing buildings are being demolished, including living environment surroundings. Materials: We measured airborne asbestos concentrations using PCM and KF-100 at research institutes, monitoring networks, subway stations and demolition sites of asbestos-containing buildings. Through this measurement data and KF-100 performance testing, we drew a conversion factor and applied it via KF-100. Finally we verified the relationship between PCM and KF-100 with statistical methods. Results: The airborne asbestos concentrations by PCM for the objects of study were less than the detection limit(7 fiber/$mm^2$) in three (20%) out of 15 samples. The highest concentration was 0.009 f/cc. The airborne asbestos concentrations by PCM in laboratories, monitoring networks, subway stations and demolition sites of asbestos-containing buildings were respectively $0.002{\pm}0.000$ f/cc, $0.004{\pm}0.001$ f/cc, $0.009{\pm}0.001$ f/cc, and $0.002{\pm}0.000$ f/cc. As a result of KF-100 performance testson rooftops, the conversion factor was 0.1958. Applying the conversion factor to KF-100 for laboratories, the airborne asbestos concentrations ratio of the two ways was nearly 1:1.5($R^2$=0.8852). Also,the airborne asbestos concentration ratio of the two ways was nearly 1:1($R^2$=0.9071) for monitoring networks, subway stations, and demolition sites of asbestos-containing buildings. As a result of independent sample t-tests, there was no distinction between airborne asbestos concentrations monitored in the two ways. Conclusions: In working areas where asbestos-containing buildings are being demolished, including living environment surroundings, quickly and accurately monitoring airborne asbestos scattered in the air around the working area is highly important. For this, we believea mutual interface of existing PCM and a real-time monitoring equipment method is possible.

Development and validation of an analytical method for nematicide imicyafos determination in agricultural products by HPLC-UVD (HPLC-UVD를 이용한 살선충제 imicyafos의 시험법 개발 및 검증)

  • Do, Jung-Ah;Park, Hyejin;Kwon, Ji-Eun;Choi, Won-Jo;Lee, Hyun-Sook;Chang, Moon-Ik;Hong, Jin-Hwan;Oh, Jae-Ho
    • Analytical Science and Technology
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    • v.27 no.5
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    • pp.234-242
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    • 2014
  • Imicyafos which is a nematicide for controlling root-knot nematodes has been registered in the Republic of Korea in 2012, and the maximum residue limits of imicyafos are set to watermelon and korean melon as each 0.05 mg/kg. Extremely reliable and sensitive analytical method is required for ensuring food safety on imicyafos residues in agricultural commodities. Imicyafos residues in samples were extracted with acetone, partitioned with hexane and dichloromethane, and then purified with florisil. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. Linear range was between 0.1~5 mg/kg with the correlation coefficient ($r^2$) 0.99997. Average recoveries of imicyafos ranged from 77.0 to 115.4% at the spiked levels of 0.02 and 0.05 mg/kg with the relative standard deviations of 2.2~9.6%. Limit of detection and quantification were 0.005 and 0.02 mg/kg, respectively. An inter-laboratory study was conducted to validate the determination method in depth, and the results were satisfactory. All of the validation results revealed that the developed analytical method in this study is relevant for imicyafos determination in agricultural commodities and will be used as an official analytical method.

Anti-listeria Activity of Lactococcus lactis Strains Isolated from Kimchi and Characteristics of Partially Purified Bacteriocins (김치에서 분리한 Lactococcus lactis 균주의 항리스테리아 활성 및 부분 정제된 박테리오신의 특성)

  • Son, Na-Yeon;Kim, Tae-Woon;Yuk, Hyun-Gyun
    • Journal of Food Hygiene and Safety
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    • v.37 no.2
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    • pp.97-106
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    • 2022
  • Listeria monocytogenes (L. monocytogenes) is one of gram-positive foodborne pathogens with a very high fatality rate. Unlike most foodborne pathogens, L. monocytogenes is capable of growing at low temperatures, such as in refrigerated foods. Thus, various physical and chemical prevention methods are used in the manufacturing, processing and distribution of food. However, there are limitations to the methods such as possible changes to the food quality and the consumer awareness of synthetic preservatives. Thus, the aim of this study was to evaluate the anti-listeria activity of lactic acid bacteria (LAB) isolated from kimchi and characterize the bacteriocin produced by Lactococcuslactis which is one of isolated strains from kimchi. The analysis on the anti-listeria activity of a total of 36 species (Lactobacillus, Weissella, Lactobacillus, and Lactococcus) isolated from kimchi by the agar overlay method revealed that L. lactis NJ 1-10 and NJ 1-16 had the highest anti-listeria activity. For quantitatively analysis on the anti-listeria activity, NJ 1-10 and NJ 1-16 were co-cultured with L. monocytogenes in Brain Heat Infusion (BHI) broth, respectively. As a result, L. monocytogenes was reduced by 3.0 log CFU/mL in 20 h, lowering the number of bacteria to below the detection limit. Both LAB strains showed anti-listeria activity against 24 serotypes of L. monocytogenes, although the sizes of clear zone was slightly different. No clear zone was observed when the supernatants of both LAB cultures were treated with proteinase-K, indicating that their anti-listerial activities might be due to the production of bacteriocins. Heat stability of the partially purified bacteriocins of NJ 1-10 and NJ 1-16 was relatively stable at 60℃ and 80℃. Yet, their anti-listeria activities were completely lost by 60 min of treatment at 100℃ and 15 min of treatment at 121℃. The analysis on the pH stability showed that their anti-listeria activities were the most stable at pH 4.01, and decreased with the increasing pH value, yet, was not completely lost. Partially purified bacteriocins showed relatively stable anti-listeria activities in acetone, ethanol, and methanol, but their activities were reduced after chloroform treatment, yet was not completely lost. Conclusively, this study revealed that the bacteriocins produced by NJ 1-10 and NJ 1-16 effectively reduced L. monocytogenes, and that they were relatively stable against heat, pH, and organic solvents, therefore implying their potential as a natural antibacterial substance for controlling L. monocytogenes in food.

Review of Remote Sensing Studies on Groundwater Resources (원격탐사의 지하수 수자원 적용 사례 고찰)

  • Lee, Jeongho
    • Korean Journal of Remote Sensing
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    • v.33 no.5_3
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    • pp.855-866
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    • 2017
  • Several research cases using remote sensing methods to analyze changes of storage and dynamics of groundwater aquifer were reviewed in this paper. The status of groundwater storage, in an area with regional scale, could be qualitatively inferred from geological feature, surface water altimetry and topography, distribution of vegetation, and difference between precipitation and evapotranspiration. These qualitative indicators could be measured by geological lineament analysis, airborne magnetic survey, DEM analysis, LAI and NDVI calculation, and surface energy balance modeling. It is certain that GRACE and InSAR have received remarkable attentions as direct utilization from satellite data for quantification of groundwater storage and dynamics. GRACE, composed of twin satellites having acceleration sensors, could detect global or regional microgravity changes and transform them into mass changes of water on surface and inside of the Earth. Numerous studies in terms of groundwater storage using GRACE sensor data were performed with several merits such that (1) there is no requirement of sensor data, (2) auxiliary data for quantification of groundwater can be entirely obtained from another satellite sensors, and (3) algorithms for processing measured data have continuously progressed from designated data management center. The limitations of GRACE for groundwater storage measurement could be defined as follows: (1) In an area with small scale, mass change quantification of groundwater might be inaccurate due to detection limit of the acceleration sensor, and (2) the results would be overestimated in case of combination between sensor and field survey data. InSAR can quantify the dynamic characteristics of aquifer by measuring vertical micro displacement, using linear proportional relation between groundwater head and vertical surface movement. However, InSAR data might now constrain their application to arid or semi-arid area whose land cover appear to be simple, and are hard to apply to the area with the anticipation of loss of coherence with surface. Development of GRACE and InSAR sensor data preprocessing algorithms optimized to topography, geology, and natural conditions of Korea should be prioritized to regionally quantify the mass change and dynamics of the groundwater resources of Korea.

Residue Patterns of Indoxacarb and Thiamethoxam in Chinese Cabbage(Brassica campestris L.) Grown under Greenhouse Conditions and Their Estimated Daily Intake (비닐하우스 재배 얼갈이배추 중 Indoxacarb와 Thiamethoxam의 잔류특성 및 식이섭취량)

  • Lee, Eun-Young;Kim, Dae-Kyu;Park, In-Young;Noh, Hyun-Ho;Park, Young-Soon;Kim, Tae-Hwa;Jin, Chung-Woo;Kim, Kwang-Ill;Yun, Sang-Soon;Oh, Sang-Kyun;Kyung, Kee-Sung
    • Korean Journal of Environmental Agriculture
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    • v.27 no.1
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    • pp.92-98
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    • 2008
  • This experiment was carried out to investigate the residue patterns of two insecticides, indoxcarb and thiamethoxam, commonly used for Chinese cabbage, under greenhouse conditions. The pesticides were sprayed onto Chinese cabbage at the recommended dose and double of the recommended dose 10 days before the prearranged harvest and then sampling was done at 0.17, 1, 2, 3, 4, 5, 6, 8, 10, and 12 days after spraying. The amounts of their residues in the crop were analyzed with an HPLC. The limit of detection(LOD) of both indoxacarb and thiamethoxam was 0.01 mg $kg^{-1}$ and mean recoveries of indoxacarb and thiamethoxam were from 97.91 to 104.36% and from 97.07 to 105.49%, respectively. Half-lives of indoxacarb and thiamethoxam were 3.4 and 2.3 days at the recommended dose and 3.3 and 3.5 days at the doubled dose, respectively. The ratios of the EDI to ADI by intake the crop harvested 10 days after spraying were less than 4% of their ADIs.

The Monitoring of Heavy Metals in Human Bloods of Middle School Students (중학생의 혈액 중 중금속 모니터링)

  • Park Hee Ra;Kim Meehye;Kwun Ki-Sung;Kim Soon Ki;Heo Su-Jeong;Kim Kwang_Jin;Yum Tae-Kyung;Choi Kwang Sik;Kim Soo Yeon
    • Journal of Food Hygiene and Safety
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    • v.20 no.2
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    • pp.83-88
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    • 2005
  • This study was conducted to estimate the contents of heavy metals including lead, cadmium, zinc, copper as well as iron status(serum iron, total iron binding capacity, feritin etc)in blood samples of middle school students(n=300). The contents of heavy metals were determined using the GF-AAS (Graphite furnace Atomic Absorption Spectrophotometer). The microwave digestion method and dilution method were compared. The dilution method showed the better recovery and detection limit than microwave digestion method. The values of toxic metals in whloe blood of boys & girls were 3.46 & 3.05 for Pb,0.063 & 0.065 for Cd respectively (ug/dL). Also the values of trace metals in serum of boys & girls were 105.9 & 92.6 for Zn, 98.3 & 99.0 for Cu respectively (ug/dL). The prevalence of iron deficiency was $7.5\%$ in 146 boys and $14.3\%$ in 156 girls. The mean values of lead in girls were higher in iron deficiency, iron deficiency anemia and anemia groups than normal group. The mean values of lead and zinc were higher in boys compared to those in girls(P<0.05), the mean values of cadmium and copper in boys were similar to those in girls. Our results of toxic metals such as Pb & Cd showed lower to CDC's(Centers for Disease Control) blood lead levels of concern for children, 10 ug/dL.

Microcystins Concentration in Fishes Collected from the Weirs of Four Rivers in Korea and Risk Assessment (국내 4대강 보에서 채집된 어류 조직에서 microcystins 농도 분석 및 위해도 평가)

  • Do-Hwan Kim;Yuna Shin;Min Jeong Park;Young-Cheol Cho
    • Korean Journal of Ecology and Environment
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    • v.55 no.2
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    • pp.120-131
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    • 2022
  • Microcystins (MCs) are cyano-toxins mainly produced by cyanobacteria in the genera of Microcystis, Anabaena, and Oscillatoria. The concentrations of MCs in the water bodies and fish tissues taken from the four weirs (Ipo, Gangjeong-goryeong, Baekje, and Juksan) in the four main rivers in Korea, and the health risk of human due to consumption of toxin-detected fish was examined. The maximum values of MCs concentration in the water samples were as follows: Juksan (3.261 ㎍ L-1), Gangjeong-goryeong (1.014 ㎍ L-1), Baekje (0.759 ㎍ L-1), and Ipo (0.266 ㎍ L-1) weirs. The MC-RR concentration was the highest among the MCs, and MC-YR was not detected. MCs of 0.222~9.808 ㎍ g-1 dry weight were detected in the liver of 3 out of 215 fishes of 16 species, and below the detection limit in muscle. As a result of comparing the feeding characteristics of the collected fishes and toxin concentrations in water and fish tissue, it was concluded that the biomagnification of MCs through the food chain did not occur. It was judged that there was no health risk due to the consumption of the fish detected the toxin, based on the amount of the fish intake of the Korean people and the allowable daily intake of MCs. However, in order to reduce the health risk due to MCs, further studies should be conducted to analyze the concentration of MCs contained in fish tissues collected at various times in the area dominated by harmful cyanobacteria to obtain data on the exposure of MCs due to fish consumption. In addition, it is necessary to establish the management guidelines for MCs in fish tissues.

Determination of $^{14}C$ in Environmental Samples Using $CO_2$ Absorption Method ($Co_2$ 흡수법에 의한 환경시료중 $^{14}C$ 정량)

  • Lee, Sang-Kuk;Kim, Chang-Kyu;Kim, Cheol-Su;Kim, Yong-Jae;Rho, Byung-Hwan,
    • Journal of Radiation Protection and Research
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    • v.22 no.1
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    • pp.35-46
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    • 1997
  • A simple and precise method of $^{14}C$ was developed to analyze $^{14}C$ in the environment samples using a commercially available $^{14}CO_2$ absorbent and a liquid scintillation counter. An air sampler and a combustion system were developed to collect HTO and $^{14}CO_2$ in the air and the biological samples simultaneously. The collection yield of $^{14}CO_2$ by the air sampler was in the range of 73-89% . The yield of the combustion system was 97%. In preparing samples for counting, the optimum ratio of $CO_2$ absorbent to the scintillator for mixing was 1:1. No variation of the specific activity of $^{14}C$ in the counting sample was observed up to 70 days after preparation of the samples. The detection limit for$^{14}C$ was 0.025 Bq/gC, which is the level applicable to the natural level of $^{14}C$. The analytical result of $^{14}C$ obtained by the present method were within ${\pm}6%$ of the relative error from the one by the benzene synthesis. The specific activity of $^{14}C$ in the air collected at Taejon during the period of October 1996 ranged from 0.26 to 0.27 Bq/gC. The specific activity of $^{14}C$ in the air collected at 1km from the Wolsong nuclear power plant a 679 MWe PHWR, was $0.54{\pm}0.03$ Bq/gC. The ranges of specific activities of $^{14}C$ in the pine needles and the vegetations from the areas around the Wolsong nuclear power plant were 0.56-0.67 Bq/gC and 0.23-1.41 Bq/gC, respectively.

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Natural Occurrence of Aflatoxigenic Aspergillus Species and Aflatoxins in Traditional Korean Fermentation Starters, Meju and Nuruk

  • Woo, So Young;Lee, Sang Yoo;Tian, Fei;Jeong, A-Yeong;Yoo, Cha Nee;Kang, Seung Yoon;Chun, Hyang Sook
    • Journal of Food Hygiene and Safety
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    • v.35 no.5
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    • pp.438-446
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    • 2020
  • Meju and nuruk (respectively soybean and malt) are traditional Korean fermentation starters that are vulnerable to contamination by harmful microorganisms such as aflatoxigenic fungi and their associated aflatoxins (AFs). In this study, Aspergillus spp. were isolated and identified from a total of 57 meju and 18 nuruk samples collected from Korean markets. Their potential aflatoxigenicity was investigated by examining the presence of three aflatoxin biosynthetic genes (aflO, aflP, and aflR) using multiplex polymerase chain reaction (mPCR) assays. Thereafter, aflatoxin production of isolates and the natural occurrence of AFs in meju and nuruk samples were analyzed by high-performance liquid chromatography (HPLC). A total of 177 Aspergillus isolates were identified and 130 isolates were obtained from meju samples. Of these, 25 isolates (19.2%) contained all three aflatoxin biosynthetic genes, and five (20%) of these isolates produced aflatoxins. Forty-seven of the Aspergillus isolates were obtained from nuruk samples, five of which (10.6%) expressed all three AF biosynthetic genes; however, none of these strains produced AFs. HPLC analysis showed that 88% (51/58) of the meju samples and 39% (7/18) of nuruk samples were not contaminated with AFs (below limit of detection). Among the isolates isolated from meju and nuruk, there were aflatoxigenic strains containing all three aflatoxin biosynthetic genes or producing aflatoxin in medium, but the frequency of aflatoxin contamination was low in the meju and nuruk samples.