• Title/Summary/Keyword: 고체상추출

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Studies on the anodic oxidation of some volatile organic halogen compounds(THM) (휘발성 할로겐 화합물(THM)의 양극 산화에 관한 연구)

  • Yoo, K.S.;Park, S.Y.;Yang, S.B.;Woo, S.B.
    • Analytical Science and Technology
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    • v.10 no.4
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    • pp.264-273
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    • 1997
  • Anodic oxidation reaction was applied to remove trihalomethanes in an aqueous solution. Each component was determined by using solid phase microextraction(SPME) fiber and GC-ECD. Anodic and cathodic compartments were separated in order to protect contaminants and connected by $KNO_3$-agar bridge. The calibration graphs of the 6 THM components were shown good linearlity from a few ppb up to a few hundreds ppb concentration level. Anodes such as platinum(Pt), titanium(Ti). zircornium(Zr), titanium metal coated with iridium(Ti-Ir), and glassy carbon coated with mixed valence ruthenium(mv Ru) were tried to remove the THMs at different potentials. The best result was obtained on the Ti-Ir anode applied 9 volts DC. The electrode could effectively remove almost all the THM components from the stirring solution within about 1.5 hours. The glassy carbon electrode coated with mixed valence ruthenium showed excellent removing effect at the begining, but the maximum removing level was remained at 60% probably due to the destruction of the electrode surface. The concentration of chloroform, however, tends to be increased due to the electrode reaction producing the component at the condition.

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Comparative Studies on K2CO3-based Catalytic Gasification of Samhwa Raw Coal and Its Ash-free Coal (삼화 원탄과 무회분탄의 촉매(K2CO3) 가스화 반응성 비교 연구)

  • Kong, Yongjin;Lim, Junghwan;Rhim, Youngjoon;Chun, Donghyuk;Lee, Sihyun;Yoo, Jiho;Rhee, Young-Woo
    • Clean Technology
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    • v.20 no.3
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    • pp.218-225
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    • 2014
  • Catalytic gasification of raw coals at mild condition is not realized yet mainly due to deactivation of catalysts via their irreversible interaction with mineral matters in coal. In this work, the gasification behavior of ash-free coal (AFC) was compared with that of the parent raw coal. In order to modify the gasification conditions, the raw coal gasified with fixed variables (water supply, space velocity, temperature, catalysts) in a fixed bed reactor. When catalysts are added by physical mixing method with coal, $K_2CO_3$ was the most effective additives for steam gasification of coal. However, the activity of ash-free coal (AFC) was much less reactive than raw coal due to high temperature extraction in a 1-methylnaphthalene under 30bar at $370^{\circ}C$ for 1 h, almost removed oxygen functional groups, and increased carbonization. The addition of $K_2CO_3$ in AFC achieved higher conversion rate at low temperature ($700^{\circ}C$). At that time, the molar ratio of gases ($H_2/CO$ and $CO_2/CO$) was increased because of water-gas shift reaction (WGSR) by addition of catalysts. This shows that catalytic steam gasification of AFCs is achievable for economic improvement of gasification process at mild temperature.

Quantitative analysis of selenium species in sea food using solid phase extraction and HPLC-ICP/MS (해산물 시료에서 solid-phase extraction 및 HPLC-ICP/MS를 이용한 셀레늄 화학종의 정량분석)

  • Kim, Eunju;Joo, Minkyu;Kwon, Hyosik;Pak, Yongnam
    • Analytical Science and Technology
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    • v.26 no.5
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    • pp.307-314
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    • 2013
  • Selenium exists in various forms of chemical species. The activity and bioavailability is strongly dependent on its chemical form and concentration. Consequently the information on each selenium species and its concentration must be exactly determined for the food we take in. In this study, selenium species in seafood were separated and quantified by RP (reversed phase) HPLC (high performance liquid chromatography) coupled with ICP-MS (inductively coupled plasma mass spectrometry) using post-column isotope dilution. $^{79}Br$, which interferes on $^{80}Se$, has mostly been removed by solid phase extraction and then mathematical correction has been applied for the more accurate correction. The experimental result for CRM (certified reference material) DOLT-4 agreed well with the certified value but each selenium species could not be compared. SeCys (selenocysteine) and SeMet (selenomethionine) were the major species detected in seafood such as belt fish, spanish mackerel, and squid that have been serving as Korean diet. The concentrations found in Korean sea food for SeCys and SeMet were in the range of 0-661.6 mg/kg and 137.3-462.7 mg/kg, respectively.

Determination of 3-phenoxybenzoic Acid in Urine and Exposure Assessment of Pyrethroid Insecticides to Human Being (요중 3-phenoxybenzoic acid 미량 분석 및 pyrethroid계 살포자 노출 평가)

  • Seo, Jong-Chul;Song, Jae-Seok;Choi, Hong-Soon
    • The Korean Journal of Pesticide Science
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    • v.11 no.2
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    • pp.87-94
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    • 2007
  • Pyrethroid insecticide have widely been used for agricultural sector and residential environments. To assess the exposure of insecticide which is absorbed through skin the analysis of urinary metabolite is essential. At present, the urinary 3-PBA was analyzed using liquid-phase extraction. But LPE have many limitations, such as long pre-treatment time and low recovery. So, this study was conducted to determine the optimum conditions for analysing 3-PBA in urine using solid phase extraction. Furthermore, this study intend to investigate the relation of concentrations of pyrethroid, deltamethrin in air and 3-PBA in urine. The optimum condition for hydrolysis was found to be done with hydrochloric acid for one hour. The recovery rates of 3-PBA were $84.6%{\pm}1.2%$, $54.8{\pm}0.9%$, $99.8{\pm}1.2%$ with XAD-2, XAD-7, XAD-16 using as the aborbents and acetone as eluents respectively. But acetonitrle and methanol gave low recovery rate and methyl cellosolve could not elute the compound. The amount of acetone for elution were 6mL, 9mL, 3mL for XAD-2, XAD-7, XAD-16 as absorbents respectively. The non-absorbed rates was $0.8{\pm}0.5%$, and $0.7{\pm}0.3%$ under XAD-16, mesh size 140-200, amount of resin 1.4g and the flow rate of eluent was 0.1mL/min. In the concentration process, we obtained 11 times higher concentration of material. The amounts of urinary 3-PBA were. The LODs of 3-PBA and deltamethrin were 0.004 mg/L, 0.038 mg/L, respectively. The further research of minute monitoring which include spray pattern, environmental condition is needed And more research about the relation between total pyrethroid exposure and urinary various metabolite are also necessary.

Preconcentration and Extraction of Copper on Activated Carbon Using 4-Amino-2, 3-dimethyl-1-phenyl-3-pyrazoline or 4-(4-methoxybenzylidenimin) thiophenole (4-Amino-2,3-dimethyl-1-phenyl-3-pyrazoline 또는 4-(4-Methoxybenzylidenimin)thiophenole을 이용한 활성탄에서의 구리의 예비 농축 및 추출)

  • Ghaedi, Mehrorang;Ahmadi, Farshid;Karimi, Hajir;Gharaghani, Shiva
    • Journal of the Korean Chemical Society
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    • v.50 no.1
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    • pp.23-31
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    • 2006
  • carbon modified methods were used for the preconcentration and determination of copper in some real samples using the flame atomic absorption spectrometry. The copper ions was adsorbed quantitatively on the activated carbon due to their complexation with 4- amino-2, 3-dimethyl-1-phenyl-3-pyrazoline (ADMPP) or 4-(4- methoxybenzylidenimin) thiophenole (MBITP). The adsorbed copper on solid phase was eluted quantitatively using small amount of nitric acid. The influence of important parameters including pH, amount of carrier, flow rate, amount of activated carbon and type and concentration of eluting agent for obtaining maximum recovery were investigated. The methods based on ADMPP and MBITP at optimum conditions is linear over concentration range of 0.05-1.5 g mL-1 and 0.05-1.2 g mL-1 of copper with correlation coefficient of 0.9997 and 0.9994 and both detection limit of 1.4 ng mL-1, respectively. The preconcentration leads to enrichment factor of 310 and break through volume of 1550 mL for both ligands. The method has a good tolerance limit of interfering ion and a selectivity that has been successfully applied for the determination of copper content in real sample such as tap, spring, river and waste water.

Determining Anti-impotence drug-like compounds in Food (식품 중 발기부전치료제 및 유사물질의 분석)

  • Choi, Dongmi;Im, Mooheg;Lee, Kyungjin;Kwon, Kwangil;Jeong, Jiyoon;Park, Gunsang;Hong, Mooki;Lee, Chulwon
    • Analytical Science and Technology
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    • v.17 no.6
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    • pp.520-526
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    • 2004
  • To determine 6 anti-impotence drug-like compounds such as sildenafil, vardenafil, tadalafil, homosildenafil, hydroxyhomosildenafil and hongdenafil in food, simultaneously, high performance liquid chromatography was applied. In the case of solid sample, it was extracted in organic solvents after homogenizing with mortar and pestle. Whereas liquid sample was just diluted in water and then extracted in organic solvents. Maximum lengths of UV for targets have been identified on photodiode array spectra. As results, vardenafil, hongdenafil, hydroxyhomosildenafil, sildenafil, homosildenafil, and tadalafil were eluted in order using $C_{18}$ column in acetonitrile containing phosphoric acid as the mobile phase. The maximum wavelength (${\lambda}_{max}$) was 216 nm for vardenafil, 233 and 282 nm for hongdenafil, 222 and 293 nm for hydroxyhomosildenafil, sildenafil and homosildenafil, and 284 nm for tadalafil. The overall recoveries were ranged from 95% to 109% and the limit of detection was about 0.04 mg/kg at signal/noise>3. Levels of targets in the selected food samples were 1.7 (hongdenafil) ~ 63 (tadalafil) mg/one dose.

Attractiveness of Host Plant Volatiles and Sex Pheromone to the Blueberry Gall Midge (Dasineura oxycoccana) (블루베리혹파리에 대한 기주식물 휘발성 물질과 성페로몬의 유인 효과)

  • Yang, Chang Yeol;Seo, Mi Hye;Yoon, Jung Beom;Shin, Yong Seub;Choi, Byeong Ryeol
    • Korean journal of applied entomology
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    • v.59 no.4
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    • pp.393-398
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    • 2020
  • The blueberry gall midge, Dasineura oxycoccana (Johnson) (Diptera: Cecidomyiidae), is an emerging pest on cultivated blueberries in Korea. To develop a sensitive tool for monitoring this pest in blueberry orchards, we compared the attractiveness of host plant volatiles and sex pheromone to D. oxycoccana adults. We performed gas chromatography-mass spectrometry (GC-MS) analysis of solid-phase microextraction (SPME)-collected volatiles that were released from blueberry ('Darrow' cultivar). The analysis revealed two major volatiles, cinnamaldehyde and cinnamyl alcohol from flowers; and three major volatiles, β-caryophyllene, germacrene D, and α-farnesene from shoots and young fruits. In field tests conducted in Gunsan, Korea in 2019, commercialized cinnamaldehyde, cinnamyl alcohol, β-caryophyllene, and α-farnesene, used singly or in quaternary combination, were unattractive to the blueberry gall midge. However, traps baited with the known sex pheromone (2R,14R)-2,14-diacetoxyheptadecane attracted significantly more males than the treatments with plant volatiles or the control. No synergistic effect was observed between sex pheromone and plant volatiles. Male D. oxycoccana were captured in the pheromone traps from May to August, with three peaks in mid-May, late June, and late July in Gunsan blueberry fields in 2020.

Determination of the Effect of Trimethylamine Reduction in Egg Yolk Following Supplementation of Laying-Hen Feed with Riboflavin

  • Park, Geon Woo;Park, Kyung Ho;Kim, Sang Gu;Lee, Sang Yun
    • Journal of Food Hygiene and Safety
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    • v.37 no.4
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    • pp.207-215
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    • 2022
  • The intensity of fishy odor in eggs, which differs depending on the poultry type and individual perception, can be due to many factors including trimethylamine (TMA) which has been identified as the main. Notably, riboflavin can increase the activity of flavin-containing monooxygenase 3, the enzyme responsible for converting TMA into odorless trimethylamine-N-oxide. This study aimed to analyze the TMA content in egg yolk, evaluate its contribution to fishy odor, and develop a method to prevent this undesired odor. Solid-phase microextraction-gas chromatography/mass spectrometry was used to detect and quantify volatile compounds in egg yolk from hens fed a standard TMA-rich diet and hens fed a riboflavin-supplemented diet. To compare the relative content of volatile substances between eggs, a correlation study was performed using an electronic nose. Higher concentration of TMA (1.06 ± 0.12 mg/kg) was detected in egg yolks obtained from hens fed a normal diet than those fed a riboflavin-supplemented diet. Overall, this study suggests that riboflavin affects the quantity and quality of volatile substances, including TMA, present in eggs and we expect these findings to improve the quality and reduce the fishy odor of eggs.

Analysis and risk assessment of formaldehyde in water from water purification plant in korea (국내 정수장 먹는 물 중 폼알데히드 함유실태 조사 및 위해성 평가 연구)

  • Chae, Hyojin;Kim, Hyun Ku;Kim, Seungki;Pyo, Heesoo;Hong, Jongki
    • Analytical Science and Technology
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    • v.22 no.5
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    • pp.386-394
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    • 2009
  • Formaldehyde is used in lether manufacture, a dry plate and an explosive. It is by-product of ozonizing process in filtration plant. The effects of exposure are eye pruritus, tickle, runing nose, blocking nasal passages and headache. It also makes a dried throat and causes inflammation. It is classified as B1 group for inhalation by US. EPA, which can cause cancer in human. For analysis of formaldehyde, formaldehydes-DNPH derivative was extracted with solid cartridge and was analyzed by High Performance Liquid Chromatography/Diode Array Detector (HPLC/DAD). The detection limit was $3{\mu}g/L$ and the recoveries were 72.3~109.1% (RSD 2.9~11.5%). Water samples were collected in four Korean rivers, four times per year seasonally for 10 years from 1998 to 2007. The monitoring results were 48.8% (630/1291), $5.15{\sim}101.9{\mu}g/L$ in purified water. Because of non-carcinogen in drinking water, hazard index is calculated with RfD. Results of excess cnacer risk was below 1 and was considered as safe value.

The analysis of pesticide residue in leafy vegetables using the modified QuEChERS pre-treatment methods (QuEChERS 시료 처리법을 활용한 엽채류 중 잔류농약분석)

  • Kim, Yang-Hyeon;Hong, Su-Myeong;Son, Kyung-Ae;Lee, Ju-Young;Min, Zaw Win;Kwon, Hye-Young;Kim, Taek-Kyum;Kyung, Kee-Sung
    • The Korean Journal of Pesticide Science
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    • v.16 no.2
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    • pp.121-130
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    • 2012
  • In analyzing pesticide residue, LLE (liquid liquid extraction) is generally applied as one of the existing methods, but needed quite a lot of organic solvents and analytical apparatuses for the sample pre-treatment. In addition to its long analysis time and complex analytical processes, it is required to develop a more rapid and efficient method at present. In order to establish an economic and simple pesticide residue analytical method, this study carried out a comparative experiment on the existing analytical method with a new sample pre-treatment method named QuEChERS (quick, easy, cheap, effective, rugged and safe), which extracts and refines pesticide components by directly adding solid powder into the sample. Both the two analytical methods showed favorable values of correlation coefficient ($R^2$ > 0.99) of calibration curves. In terms of the detection limit (identification limit), imidacloprid showed 0.02 mg/kg, while the rest of pesticides showed a level around 0.05 mg/kg. The results of this experiment revealed that the recovery of LLE was 92.8-100.9% and the RSD was below 2.5%. On the other hand, the recovery of QuEChERS was 92.2-101.6% and RSD was below 1.9%. As a result of comparing the amount of pesticide residue by the time between the two analytical methods by using Paired t-Test, there was no significant difference between the two analytical methods as the p-value ranged from 0.3148-0.9890. Considering the results of the two methods, the QuEChERS method had similar recovery, compared to the analytical method using the existing LLE, and the analytical time was shortened by about one fourth of that of the existing method. Moreover, since it excludes the use of harmful organic solvents like dichloromethane during the process of extraction, thus leading to protecting experimenters health and remarkably reducing the amount of disused solvents, it is judged as an echo-friendly and economic analytical method.