• Title/Summary/Keyword: method detection limit

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Residues of sulfadimethoxine in blood and liver of cultured olive flounder Paralichthys olivaceus by oral administration (Sulfadimethoxine의 경구 투여에 따른 넙치, Paralichthys olivaceus 혈액 및 간에서의 잔류량 변화)

  • Jun, Sung-Hee;Kim, Jin-Woo;Seo, Jung-Soo;Jee, Bo-Young;Park, Myoung-Ae
    • Journal of fish pathology
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    • v.25 no.2
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    • pp.95-101
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    • 2012
  • The residue levels of sulfadimethoxine (SDM) was studied after oral administration to cultured olive flounder, Paralichthys olivaceus at $20{\pm}1.0^{\circ}C$. The concentrations of SDM in the plasma and liver were determined by HPLC-UV detector after a single dosage of 400 mg/kg body weight. The average recoveries of SDM in spiked samples between 2~50 ppm were 92.24~93.62% for plasma and 88.34~91.90% for liver. Limit of detection for SDM was 0.05 ppm by using this method. Samples were taken at 1 h, 6 h, 12 h, 24 h, 48 h, 72 h, 168 h, 240 h, 336 h and 480 h post-dose. The peak plasma and liver concentrations of SDM, which attained at 1 h post-dose, was $402.64{\pm}59.66{\mu}g/ml$ and $238.18{\pm}54{\mu}g/g$, respectively. Thereafter, it's elimination from both tissues was considerably faster following process of time. Their concentrations of SDM were not measurable at 480 h post-dose. Based on this results, dosage and withdrawal times for SDM could be used when it is prescribed with SDM in olive flounder.

Determination of Amitrole in Water Samples by Evaporation and GC/MS (증발법과 GC/MS를 이용한 수질 시료 중의 Amitrole의 분석법 연구)

  • Yoon, So Hee;Hong, Ji Eun;Pyo, Hee Soo;Park, Song Ja
    • Analytical Science and Technology
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    • v.16 no.6
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    • pp.483-487
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    • 2003
  • Amitrole is well-known as a non-selective herbicide and it is able to cause contamination of driking water as well as pollution of ground water and surface water. However, it is difficult to extract from water because it has a high solubility for water whereas a low solubility for general organic solvents. This method is described for the determination of amitrole in water samples by GC/MS. After evaporation of 10 mL water sample by a vacuum evaporator, amitrole was derivatized with isobutyl chloroformate (iso-BCF) on room temperature for 15~20 min. As a result, the sensitivity for GCfMS was improved as N-isobutoxycarbonyl amitrole derivative was formed. The linearity of the calibration curve showed good as 0.997. The recoveries were obtained more than 94.9% and relative standard deviations were less than 2.8% at $1.0{\mu}g/L$, $10.0{\mu}g/L$ and $100.0{\mu}g/L$. The limit of detection showed $0.1{\mu}g/L$ with a signal-to-noise ratio (S/N) of 3.

Differential Pulse Voltammetric Determination of Iron(III) Ion with a Sodium Dodecyl Sulfate Modified Glassy Carbon Electrode (시차펄스전압전류법에서 도데실황산나트륨이 수식된 유리탄소전극에 의한 선택성 있는 철(III) 이온의 정량)

  • Ko, Young Chun;Kim, Jin Ah;Chung, Keun Ho
    • Analytical Science and Technology
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    • v.10 no.6
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    • pp.427-432
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    • 1997
  • A selective method for the determination of iron(III) ion with a sodium dodecyl sulfate(SDS) modified glassy carbon electrode was proposed. It was based on the electrostatic attraction and complexation of the SDS modifier, $(DS^-)_n-Fe^{3+}$. The determination of iron(III) ion was performed by a differential pulse voltammetry(DPV), and the reduction peak potential of $(DS^-)_n-Fe^{3+}$ was +0.466(${\pm}0.002$)V vs. Ag/AgCl. For the determination of iron(III) ion, a linear calibration curve was obtained within the iron(III) ion concentration range of $0.50{\times}10^{-5}{\sim}10{\times}10^{-5}mol/L$, and the detection limit was $0.14{\times}10^{-5}mol/L$. $Cu^{2+}$, $Ni^{2+}$, $Co^{2+}$, $Pb^{2+}$, $Zn^{2+}$, and $Mn^{2+}$ showed little or no effect on the determination of iron(III) ion, respectively. But, ion such as each $CN^- $ and $SCN^-$ interfered seriously.

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Monitoring of Butyltin Compounds in PVC Food Packaging - Determination of Butyltin Compounds in PVC Wrap and Gasket for Food Packaging by GC/MS (식품용 염화비닐수지제 기구 및 용기.포장 중 부틸주석화합물의 모니터링 - GC/MS를 이용한 염화비닐수지제 식품용 랩 및 가스킷 재질 중 부틸주석화합물 잔류량 분석)

  • Sung, Jun-Hyun;Yoon, Hae-Jung;Choi, Hyun-Cheol;Jeon, Dae-Hoon;Eom, Mi-Ok;Kim, Hyung-Il;Park, Na-Young;Lee, Eun-Joon;Lee, Young-Ja
    • Korean Journal of Food Science and Technology
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    • v.39 no.6
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    • pp.715-720
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    • 2007
  • The levels of butyltin compounds in poly(vinyl chloride) (PVC) food packaging using gas chromatography/mass spectrometry (GC/MS) were monitored. The analytical method, involving the ethylation with sodium tetraethylborate, was found to be selective and sensitive for mono-n-butyltin (MBT), di-n-butyltin (DBT), and tri-n-butyltin (TBT), validated by a $0.005\;{\mu}g/mL$ limit of detection (LOD), an $R^2>0.999$ for linearity, and >90% of recovery, respectively. Finally, none of the commercial food wraps and gaskets showed detectable levels of butyltin compounds.

Exposure Assessment of N-nitrosamines in Foods (식품을 통한 니트로사민 노출량 평가)

  • Jo, Cheon-Ho;Park, Hee-Ra;Kim, Dong-Sul;Lee, Kwang-Ho;Kim, Mee-Hye
    • Korean Journal of Food Science and Technology
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    • v.42 no.5
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    • pp.541-548
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    • 2010
  • In this study, contamination levels of 7 N-nitrosamine were investigated in processed meat products (n=51), processed fish products (n=62), salted fish pickles (n=20), and beer and malt beverages (n=21) using a GC/PCI-MS/MS method. The limits of detection (LOD) of the N-nitrosamines ranged from 0.2 to 0.5 ${\mu}g$/kg. In addition, methods were used to estimate the recovery of 7 N-nitrosamines, which ranged from 84 to 112%. N-nitrosamines were detected in 89 (58%) out of 154 samples. The exposure of an entire population group to N-nitrosamines through food intake was estimated using the average body weight of the total population and average daily food consumption, to perform risk assessment based on reports of a national health and nutrition survey. The results indicated that the daily intake of N-nitrosamines over a life time was $4.92{\times}10^{-7}$ mg/kg b.w./day. The margin of exposure (MOE) for the general population, estimated using the benchmark dose lower confidence limit 10 ($BMDL_{10}$) of N-nitrosodimethylamine, was 208,939, which was found to be safe.

Studies on Analytical Methods for N-Methylcarbamate Residues in Crops by Spectrophotometry and Gas Liquid Chromatography (작물체중(作物體中) N-Methylcarbamate계(系) 농약(農藥)의 잔류분석법(殘留分析法)에 관(關)한 연구(硏究))

  • Oh, Byung-Youl;Jeong, Young-Ho;Park, Young-Sun
    • Korean Journal of Environmental Agriculture
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    • v.1 no.1
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    • pp.14-21
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    • 1982
  • Analytical methods for residues of six N-methylcarbamate insecticides were investigated to compare the minimum detectability, recovery from several crops and feasibility of multiple residue analysis. Those methods studied in this work included spectrophotometry by diazotization and gas chromatography by N-trifluoroacetylation(TFA), pentafluorobenzylether(PFB) and dinitrophenylether (DNP) derivatization. Maximum absorbed wavelength of the diazotized MIPC, XMC, BPMC, propoxur and carbofu ran was around 460 ㎚, while that of carbaryl recorded 510 ㎚. Recovery from brown rice and apple by diazotization method ranged from 80 to 120% and minimum detectable limits were 0.03 to 0.05 ppm in 50 g of the sample. Minimum detectability of PFB derivatives by gas chromatography was superior to TFA and DNP derivatives. DNP derivatives showed the longest retention time among the given derivatives. Recovery from crops by gas chromatographic met hod ranged 74 to 94%, 78 to 93%, and 85 to 99% in brown rice, rice straw and apple, respectively. Limit of detection was 0.01 ppm for TFA, 0.005 ppm for PFB and 0.02 ppm for DNP derivatives in 50 g of the crop samples.

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Concentration of Arsenic in Rice Plants and Paddy Soils in the Vicinity of Abandoned Zinc Mine (폐광산 인근 논토양과 수도의 비소함량 조사)

  • Kim, Chan-Yong;Park, Man;Lee, Dong-Hoon;Choi, Choong-Lyeal;Kim, Kwang-Seop;Choi, Jung;Seo, Young-Jin
    • Applied Biological Chemistry
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    • v.45 no.3
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    • pp.152-156
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    • 2002
  • Soils near abandoned zinc mines were known to be contaminated with arsenic-rich mining by-products. To examine the potential impacts of arsenic- contaminated soils on plant growth, surface soils were subjected to sequential extraction. Results revealed that 54% and 74% total As and 74% total extractable As were bound to iron hydrous oxide, and water soluble fraction was below detection limit. Arsenic faction extracted using the Koran standard method(dissolution of metals via treatment of 1 N HCI) was strongly correlated with the Fe-bound As fraction ($r^2=0.884**$). Arsenic level in rice plant roots was the highest with a maximum value of 154.9 mg/kg, whereas it was below 0.6 mg/kg in grains. Arsenic level in rice plant roots was strongly correlated with those of Al-bound As ($r^2=0.821**$) and 1N HCI-extractable As levels ($r^2=0.801**$).

A Correlation Study between the Environmental, Personal Exposures and Biomarkers for Volatile Organic Compounds (대기 중 휘발성유기오염물질의 환경, 개인 및 인체 노출의 상관성 연구)

  • Jo, Seong-Joon;Shin, Dong-Chun;Chung, Yong;Breysse, Patrick N.
    • Environmental Analysis Health and Toxicology
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    • v.17 no.3
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    • pp.197-205
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    • 2002
  • Volatile organic compounds (VOCs) are an important public health problem throughout the world. Many important questions remain to be addressed in assessing exposure to these compounds. Because they are ubiquitous and highly volatile, special techniques must be applied in the analytical determination of VOCs. Personal exposure measurements are needed to evaluate the relationship between microenvironmental concentrations and actual exposures. It is also important to investigate exposure frequency, duration, and intensity, as well as personal exposure characteristics. In addition to air monitoring, biological monitoring may contribute significantly to risk assessment by allowing estimation of absorbed doses, rather than just the external exposure concentrations, which are evaluated by environmental and personal monitoring. This study was conducted to establish the analytic procedure of VOCs in air, blood, urine and exhaled breath and to evaluate the relationships among these environmental media. The subjects of this study were selected because they are occupationally exposed to high levels of VOCs. Environmental, personal, blood, urine and exhalation samples were collected. Purge & trap, thermal desorber, gas chromatography and mass selective detector were used to analyze the collected samples. Analytical procedures were validated with the“break through test”, 'quot;recovery test for storage and transportation”,“method detection limit test”and“inter-laboratory QA/QC study”. Assessment of halogenated compounds indicted that they were significantly correlated to each other (p value < 0.01). In a similar manner, aromatic compounds were also correlated, except in urine sample. Linear regression was used to evaluate the relationships between personal exposures and environmental concentrations. These relationships for aromatic and halogenated are as follows: Halogen $s_{personal}$ = 3.875+0.068Halogen $s_{environmet}$, ($R^2$= .930) Aromatic $s_{personal}$ = 34217.757-31.266Aromatic $s_{environmet}$, ($R^2$= .821) Multiple regression was used to evaluate the relationship between exposures and various exposure deter-minants including, gender, duration of employment, and smoking history. The results of the regression model-ins for halogens in blood and aromatics in urine are as follows: Halogen $s_{blood}$ = 8.181+0.246Halogen $s_{personal}$+3.975Gender ($R^2$= .925), Aromatic $s_{urine}$ = 249.565+0.135Aromatic $s_{personal}$ -5.651 D.S ($R^2$ = .735), In conclusion, we have established analytic procedures for VOC measurement in biological and environmental samples and have presented data demonstrating relationships between VOCs levels in biological media and environmental samples. Abbreviation GC/MS, Gas Chromatography/Mass Spectrometer; VOCs, Volatile Organic Compounds; OVM, Organic Vapor Monitor; TO, Toxic Organicsapor Monitor; TO, Toxic Organics.

Solvent Extraction of Trace Amount of Ni(II) in Sea Water by using Salen[N,N'-bis(salicylidene)ethylenediamine] (Salen[N,N'-bis(salicylidene)ethylenediamine]을 이용한 해수 중 극미량 니켈의 용매추출)

  • In, Gyo;Choi, Jong-Moon;Kim, Young-Sang
    • Analytical Science and Technology
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    • v.17 no.6
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    • pp.481-488
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    • 2004
  • Solvent extraction of Ni(II) into a chloroform by using salen[N,N'-Bis (salicylidene)-ethylenediamine] as a ligand has been studied. Salen was synthesized from ethylenediamine and salicylaldehyde by simple condensation reaction in an ethanol. Salen formed a 1 : 1 complex with Ni(II) and its extraction constant was $10^{5.12}$. For the determination of Ni(II) in sea water samples, some experimental conditions such as pH of solution, amount of salen, acid type and concentration for back extraction, extraction time, and influence of foreign ions were optimized by using a synthetic sea water. The sea water of which the composition was similar to a natural sea water was synthesized in this laboratory. Trace Ni(II) was extracted into the chloroform in the weak basic solution above pH 8. And the nickel could be quantitatively extracted with the concentration of salen higher than $1.2{\times}10^{-4}mol/L$. This concentration was more than 180 times of Ni(II) in the solution with a mole ratio. Real samples of Korean coastal sea water were analyzed under optimized conditions. Even though Ni(II) was not detected in these samples. Recoveries more than 98% were obtained in the samples which 40 ng/mL of Ni(II) was spiked. And detection limit of proposed method was 1.3 ng/mL. From these results, it could be known that salen of this type would be applied for the determination of trace metals as an organic chelating reagent.

A Study on the Application of Sulfur-Free Odorant for LPG Fuel (LPG 연료용 비황분계 부취제의 적용성 연구)

  • Kim, Jae-Kon;Yim, Eui Soon;Jung, Choong-Sub
    • Journal of the Korean Institute of Gas
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    • v.18 no.5
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    • pp.52-59
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    • 2014
  • In general, sulfur containing odorants are added to fuel gases, such as LPG, and city gas, to prevent gas poisoning, ignition, explosion, or other accident caused by fuel gases, and to enable immediate and easy detection of fuel-gas leakage by emitting an offensive smell. In this study, sulfur free odorant for low sulfur fuel and prevention of metal corrosion were developed to replace current sulfur containing odorant for gas fuel. They were selected from 12 odorant containing non-sulfur organic compounds and evaluated by odor olfactory method (odor quality, odor intensity). Finally, selected mixture odorants were methyl isovalerate, methyl acrylate, 2-ethyl-3-methyl pyrazine with blending ratio of 50% : 40% : 10%. Final Sulfur free odorant was added 40 wt ppm in LPG fuels and evaluated fuel quality characteristics, metal corrosion test and long term stability of LPG fuel. It were limit in current LPG fuel standard in fuel quality characteristics. Final Sulfur free odorant also had no influence on metal corrosion and long term stability test with 60 days by adding in LPG fuels. Finally, they were shown to be warning agent candidates to reduce sulfur content and metal corrosion for LPG fuel.