• Journal of Korean Society for Atmospheric Environment
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• v.7 no.1
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• pp.1-16
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• 1991

In this study, sampling and analytical procedures were evaluated for the determination of ambient levels of atmospheric PAH, both in gaseous and particulate phase. The method involves low-volume sampling and Soxhlet extraction of the filters and Tenax absorbent, followed by a clean-up stage using a silica column prior to analysis by reversed-phase HPLC with wavelength programmable fluorescence and UV detection. A total of 18 PAH were identified and quantified, all of which have been of environmental concern. In order to validate the methodology and to ensure compatibility of the results, the analytical method used for the determination of PAH was evaluated with respect to the efficiencies of extraction and clean-up procedure, HPLC separation, and lower limits of detection. In addition, substrate dependency of PAH recovery was investigated for the two types of fiters, i.e. glass fiber and PTFE filters.

• Analytical Science and Technology
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• v.13 no.4
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• pp.484-493
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• 2000

The simultaneous analysis of alkylphenols, chlorophenols and bisphenol A in biota samples was performed by gas chromatography-mass spectrometry-selected ion monitoring mode. The phenols were extracted from sample with organic solvent and Forisil and Silica columns for clean-up procedure were compared. Recovery studies were performed at 1-ppm level of phenols added to each biota sample. Their recoveries ranged between 83 and 116% with coefficient of variations of 2.4-11.9%. To improve the detection limits of phenols, trimethylsilyl (TMS) derivatization was applied. The gas chromatographic properties of free phenols and TMS derivatized phenols were also investigated.

• Journal of Soil and Groundwater Environment
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• v.9 no.3
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• pp.20-26
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• 2004

In-situ photolysis is one of the most promising ways to clean up a soil contaminated with 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD). This study focuses on the mathematical description and model development of the convective upward transport of an organic solvent driven by evaporation and photodecomposition at the surface as the major transport mechanism in the clean up process. A finite-element-based numerical model was proposed to incorporate effects of multiphase flow on the distribution of each fluid, gravity as a driving force, and the use of van Genutchen equation for more accurate description of k-S-p relations. This paper presents results of extensive numerical calculations conducted to investigate the various parameters that play a role in the solvent migration through a laboratory-scale unsaturated soil column. The numerical results indicate that gravity affects significantly on the fluids distribution and evaporation for highly permeable soils. The soil texture has a profound influence on the fluid saturation profile during evaporation process. The amount of solvent convective motion increases with increasing evaporation rates and decreasing initial water saturation. Simulations conducted in this study have shown that the developed model is very useful in analyzing the effects of various parameters on the convective migration of an organic solvent in the soil environments.

• Bulletin of the Korean Chemical Society
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• v.26 no.12
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• pp.1996-2000
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• 2005

Headspace hanging drop liquid phase micro-extraction (HS-HD-LPME) is studied as a novel solvent-based sample pretreatment method for floral volatile aroma compounds. This paper reports on application of the HSHD- LPME combined with GC-MS for the analysis of linalool component emitted from evening primrose flowers. The effect of several variables on the method performance was investigated. Additionally, the separation of enantiomers on a cyclodextrin capillary column was performed to identify chirality of (−)-linalool component. Since the unsurpassed volume of a few micro-liters of solvent is used, there is minimal waste or exposure to toxic organic solvents. This method enables to combine extraction, enrichment, clean-up, and sample introduction into a single step prior to the chromatographic process.

• Journal of Food Hygiene and Safety
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• v.8 no.1
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• pp.1-8
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• 1993

육류중에 잔류하는 항생물질 및 항균제를 검출하기 위해 본 실험에서는 3종의 균주 Bacillus subtilis ATCC 6633, Micrococcus luteus ATCC 9341, BAcillus cereus var. mycoides ATCC 11778을 사용하여 실험하였다. 시료의 clean-up은 항생·항균제의 물리화학적 성질을 고려하여 우선 McIlvaine buffer를 가하여 homogenize하고 hexane으로 defatting 시킨 후, chloroform으로 추출한 액과 Sep-Pak C18과 Bakerbond SPE carboxylic acid column에 흡착시킨 후 추출한 액을 각각 시험용액 A, B, C,로 하였다. 각 test solution을 paper disk를 사용하여 함균 배지에 올려놓고 overnight culture 후 inhibition pattern을 통해 여러 종류의 항생·항균제를 계통적으로 검출하였다. 본 실험에서 macrolide계와 tetracycline계 등은 0.1ppm 이하의 detection limit을 보였으며, penicillinrP는 0.001ppm이하의 높은 detection limit을 나타내므로서 시료중에 잔류하는 극미량까지도 검출할 수 있었다. 본 방법은 식육중의 잔류 항생·항균제를 동시에 간단하게 계통적으로 분류하는데 있어 좋은 방법이라고 생각되며 항생·항균제의 체계적인 1차 screening 수단으로서 유용한 방법이라 사료된다.

• Archives of Pharmacal Research
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• v.15 no.2
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• pp.109-114
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• 1992

For the risk assessment of human exposure to volatile halogenated hydrocarbons, a dynamic purge trap/on-column cryofocusing method using capillary gas chromatograph-$^{63}Ni$ electron capture detector and thermal desorption unit was applied to analyze the free forms, metabolites of 1, 1, 2-trichloroethylene and 1, 1, 2, 2-tetrachloroethylene. The urine sample was diluted with distilled water, hydrolyzed and sealed. Then the inert gas was infused to purge out free 1, 1, 2-trichloroethylene, free 1, 1, 2, 2-tetrachloroethylene and urichloroethanol. These compounds were trapped to $Tenax^R$ / GC-gas trap device throughout clean up tube. Being undertectable to gas chromatograph directly, trichloroacetic acid was methyl esterificated and trapped in the manner above mentioned. The optimal incubation time to get best recovery of methyl ester was 4 hours at $60^circ$C. The concentrations of free volatile halogenated hydrocarbons and their metabolites in urine were obtained of free volatile halogenated hydrocarbons and their metabolites in urine were obtained from 5 healthy volunteers. This analytical method is expected to make the biological monitoring more precise and convenient.

• Korean Journal of Food Science and Technology
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• v.36 no.1
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• pp.158-161
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• 2004

To determine rapid and reliable analytical method for ochratoxin A detection in cereal-based Korean traditional foods, ochratoxin A content was measured by high-performance liquid chromatography (HPLC) with immunoaffinity column clean-up. Recoveries of ochratoxin A in tested samples ranged from 68.4 to 85.3%. Occurrences of ochratoxin A were 15, 10, and 5% for Kochujang, Deonjang, and Kanjang, respectively. None was detected in Sunsik (mixed cereals). Average levels of ochratoxin A ranged from $0.5\;to\;1.3{\mu}g/kg$, lower than maximum residue level of $5-50{\mu}g/kg$ of ochratoxin A recorded in foreign food code.

• Bulletin of the Korean Chemical Society
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• v.26 no.4
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• pp.529-536
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• 2005

Measurement of toxicologically relevant polychlorinated biphenyl (PCB) congeners such as non-ortho(IUPAC#) 77, 81, 126, 169 and mono-ortho 105, 114, 118, 123, 156, 157, 189 and di-ortho 170, 180 and polybrominated diphenyl ethers (PBDEs) such as 47, 66, 85, 99, 100, 138, 153, 154 in environmental samples become almost mandatory in several countries now. However, most of the available methods involve expensive instrumentations such as HRGC-HRMS or ECNI-LRMS, apart from expensive extraction and clean-up (with large volume of solvents) steps. A method has been devised combining the analytical separation power of PYE [2-(1-pyrenyl)ethyldimethysilylated silica] column HPLC and high-resolution gas chromatographic techniques including micro-electron capture detection (ECD) and two dimensional gas chromatograpy-ECD techniques to determine these eco-toxic substances at parts-per-trillion (ppt) levels. This combination resolves co-elution of congeners that occur in disproportionate ratios (e.g. CB-110 and -77) and allows accurate congener-specific determination of target compounds. This method is cost effective as it requires only hexane, that in small quantities (10 mL) and GC-ECD. The elution and analysis time are optimized to less man hours. This method is effectively utilized in the analysis of co-planar PCBs and PBDEs from archived solvent extracts of samples previously analyzed for pesticides and PCBs. Structure based separation of contaminant classes improves GCECD determination at ppt levels.

• Preventive Nutrition and Food Science
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• v.8 no.4
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• pp.301-305
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• 2003

This study was conducted to develop an HPLC method for determining vitamin B$_{12}$ in fortified foods which has typically been determined by microbiological assays according to AOAC and Korean Food Code approved methods. Vitamin B$_{12}$ (cyanocobalamin) was determined by reversed-phase HPLC with a triple column and UV/VIS dectector (550 nm) using the column switching technique after extraction with 5 mM potassium phosphate solution by sonication without a clean-up procedure. The recovery of spiked samples and limit of detection (LOD) by HPLC were 78.6 ∼107.5 % and 2 ppb ($\mu\textrm{g}$/kg), respectively. The LOD of the microbiological assay (MBA) was much lower than that of HPLC. The concentrations of vitamin B$_{12}$ analyzed in all tested samples (n=12) confirmed compliance with declared label claims. The range of recovery ratio by the HPLC method when compared to the microbiological assay was 76.2 ∼140.0 %. There was not significant difference between the HPLC and MBA methods (p < 0.01) with r=0.9791 and linear regression y=0.9923x-0.04. The HPLC method for determining vitamin B$_{12}$ using the column-switching technique appears to be suitable for determining vitamin B$_{12}$ concentrations above 1 $\mu\textrm{g}$/100 g in fortified foods.ied foods.

• Korean Journal of Environmental Agriculture
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• v.18 no.2
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• pp.135-139
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• 1999

A new effective and economic method was developed, removing interferences such as chlorophyll and lipid from leaves with small amounts of reagents and solvents in order to analyse PAHs(Polycyclic Aromatic Hydrocarbons). The extract from a soxhlet containing $4{\sim}5g$ of leaves and 100ml of dichlormethane and refluxed for 20 hrs was concentrated and eluted with 60ml of a hexane:dichloromethane (1:1) mixture through a column of 9mm wide inner diameter and 130mm long, packed from the bottom with 2.5g of $Al_2O_3$, 1.5g of $SiO_2$and 2g of anhydrous $Na_2SO_4$. The eluent was concentrated and loaded on a GPC column of 20mm wide inner diameter and 280mm long, packed with 12g of Bio-beads. The column was washed with 37ml of the hexane:dichloromethane(1:1) mixture. Another 43ml of the mixture was eluted as a PAH fraction and collected. This eluent was concentrated under gentle nitrogen to $50{\mu}l$ and analysed using GC-MS. The recoveries, obtained by comparing with the amounts of the internal standards of deuterated PAHs were $43.3{\sim}107.5%$(RSD $2.2{\sim}9.5%$).