• Proceedings of the Korean Society for Food Science of Animal Resources Conference
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• 2005.10a
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• pp.196-203
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• 2005

축산식품 고기내의 잔류항생물질을 신속하고 간편하고 정확하게 분석하기 위한 시험법 개발 을 목적으로 하였다. 축산식품내의 일반적인 잔류항생물질에 대한 지금까지의 분석법으로는 Bioassay법, TLC법, ELISA법, GC법 및 HPLC법 등이 있지만 Streptomycin/Dihydro streptomycin, Neomycin에 대한 HPLC법은 거의 확립되어 있지 않은 실정이다. 우리나라의 공인 검사법으로는 Bioassay법 및 HPLC법 등이 있지만 그러나 지금까지의 방법으로는 검출감도가 낮은 것이 큰 문제점으로 되어 왔다. 본 연구에서는 DST에 대한 HPLC법에 대한 보고한 P. Edder 방법 중에 clean-up과정 및 이동상 조건을 대폭 수정하여 DST의 분리 및 검출감도를 낮추려고 시도하였다. 본 연구에 사용된 유도체화 장치 Post-Column Derivatization Instrument PCX 5100 (Pickering Laboratories, Inc.)의 컬럼온도는 $40^{\circ}C$, 오븐온도 $55^{\circ}C$, reagent 유속 0.6ml/min mobile phase 유속 0.8ml/min으로 검출기는 형광검출기를 이용하여 DST 검출에 대해 만족할 만한 결과를 얻었다. 이때의 분석소요시간은 약 15분이었다. 표준시료 DST의 검량선은 넓은 농도범위(0.02${\sim}$1.0ppm)에서 양호한 직선성을 나타냈다. 본 시험법에 의한 검출한계는 limit of detection (LOD)은 0.02ppm이었으며, 적어도 고기에서의 MRL이 0.6ppm임을 감안하면 DST를 정량적으로 정도 좋게 측정할 수 있다는 것을 확인했다. 상기의 조건하에서 실제시료인 고기에 표준 DST를 1ppm을 spiking한 후 SPE상에서 SCX(Strong cation exchange column)을 통한 clean-up과정을 거친 후의 DST의 limit of quantification(LOQ)는 약 0.47ppm이었으며, 이에 대한 회수율은 97.7%(n= 8)를 나타냈다. 실제 codex에서 권장한 고기의 MRL이 0.6ppm인 점을 감안하면 codex 권고치에 도달할 수 있는 것으로 판단되었다. 따라서 본 연구에서 개발된 시험법은 지금까지 국내적으로 DST에 대한 시험법이 확립되어 있지 않은 것으로 이와 아울러 간편한 parallux와 병용해 DST에 대한 정량 및 정성 분석을 유도체화 장치 및 형광검출기를 이용해 잔류항생물질 DST에 대한 분석시험법의 개발이 가능하다고 여겨진다.

• Proceedings of the Korean Society for Food Science of Animal Resources Conference
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• 2005.10a
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• pp.310-316
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• 2005

축산식품(우유)내의 잔류항생물질을 신속하고 간편하고 정확하게 분석하기 위한 시험법 개발을 목적으로 하였다. 축산식품내의 일반적인 잔류항생물질에 대한 지금까지의 분석법으로는 Bioassay법, TLC법, ELISA법, GC법 및 HPLC법 등이 있지만 Streptomycin/dihydrostreptomycin, neomycin에 대한 HPLC법은 거의 확립되어 있지 않은 실정이다. 우리나라의 공인 검사법으로는 Bioassay법 및 HPLC법등이 있지만 그러나 지금까지의 방법으로는 검출감도가 낮은 것이 큰 문제점으로 되어 왔다. 본 연구에서는 STP에 대한 HPLC법에 대한 보고한 Edder 방법 중에 clean-up 과정 및 이동상 조건을 대폭 수정하여 STP의 분리 및 검출감도를 낮추려고 시도하였다. 본 연구에 사용된 유도체화 장치 Post-Column Derivatization Instrument PCX 5100 (Pickering La-boratories, Inc.)의 컬럼 온도는 $40^{\circ}C$, 오븐온도 $55^{\circ}C$, 유도체화 용매 유속 0.6ml/min 이동상 유속 0.8ml/min으로 검출기는 형광검출기를 이용하여 STP 검출에 대해 만족할 만한 결과를 얻었다. 이때의 분석소요시간은 약 15분이었다. 표준시료 STP의 검량선은 넓은 농도범위(0.02${\sim}$1.0ppm)에서 양호한 직선성을 나타냈다. 본 시험법에 의한 검출한계는 limit of detection(LOD)은 0.02ppm이었으며, 적어도 우유에서의 MRL이 0.6ppm임을 감안하면 STP를 정량적으로 정도 좋게 측정할 수 있다는 것을 확인했다. 상기의 조건하에서 실제시료인 우유에 표준 STP를 0.5ppm을 spiking한 후 SPE상에서 SCX(Strong cation exchange column)을 통한 clean-up과정을 거친 후의 STP의 limit of quantification(LOQ)는 약 0.44ppm이었으며, 이에 대한 회수율은 89.7${\pm}$2.3%(n=6)를 나타냈다. 실제 CODEX에서 권장한 우유의 MRL이 0.6ppm인 점을 감안하면 CODEX권고치에 도달할 수 있는 것으로 판단되었다. 따라서 본 연구에서 개발 된 시험법은 지금까지 국내적으로 STP에 대한 시험법이 확립되어 있지 않은 것으로 이와 아울러 간편한 parallux와 병용해 STP에 대한 정량 및 정성 분석을 유도체화 장치 및 형광검출기를 이용해 잔류항생물질 STP에 대한 분석시험법을 개발하였다.

• Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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• 2004.04a
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• pp.73-76
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• 2004

Rusted iron could retain activity to redox-sensitive pollutants in batch reactor. Flow-through columns packed with permeable reactive iron filings (Fe$^{0}$ ) between soil and sand layers were used to evaluate the applicability of bio-enhanced iron barriers to treat explosives-contaminated groundwater. One column was bioaugmented with municipal anaerobic sludge to evaluate the enhancement of biodegradation. Military contaminants (RDX, HMX, TNT, 2,4DNT, 2,6DNT), which coexist in soils at military sites, were completely removed in the bioaugmented Fe$^{0}$ layer after 8 months of operation. Overall, this research suggests that Fe$^{0}$ barriers can effectively clean up groundwater contaminated with military explosives, and that treatment efficiency can be enhanced by bioaugmentation.

• Journal of Food Hygiene and Safety
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• v.9 no.2
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• pp.89-94
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• 1994

A simple, safe, and sensitive gas chromatographic method using packed column and electron capture detector to analyze 2, 4-D herbicide in imported lemon, grapefruit, and orange was described and its usefulness evaluated. In this scheme of analysis the acid herbicide was converted into its alkyl esters by an one-step reaction prior to analysis. The herbicide in the fruits was extracted with ethyl acetate and partitioned against dichloromethane for purification, and the extracts finished partitioning were derivatized with alcohol, using sulfuric acid as a catalyst to form the corresponding alkyl derivatives. The analytical scheme studiedwas found to be applicable for the herbicide in the fruits without a column clean-up procedure. The mean recoveries of the herbicide for lemon samples fortified at 0.1 mg/kg and 1.0 mg/kg were 93% and 95%, respectively. The detection limit was 0.5 $\mu\textrm{g}$/kg for 2.4-D methyl ester.

• Journal of Food Hygiene and Safety
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• v.5 no.4
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• pp.213-217
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• 1990

A simple and practical method for the determination of caffeine in coffee, black tea and green tea was studied. The analysis of caffeine was performed by reverse phase high perfomance liquid chromatography using a ${\mu}-Bondapak$ C18 column at isocratic condition with methanol-acetic acid-water (20: 1: 79) on UV detector at 280 nm. The extraction and clean-up of caffeine in sample is based on combing a simple pretreatment with the use of a Sep-Pak Alumina A cartridge. The average recoveries of caffeine from several samples were 95.2 -101.3%, the relative standard deviation for the whole procedure was 0.10 ~ 0.62%, and the detection limit of caffeine in sample solution was about $0.1\;\mu\textrm{g}\;per\;ml$.

• Analytical Science and Technology
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• v.6 no.3
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• pp.283-288
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• 1993

The solvent extraction and clean up processes for the gas chromatographic determination of muarimol pesticide residues in apples were investigated and examined the changes of residual concentration with the passage of time. The extracted pesticide with methanol were partitioned with dichloromethane after adding sodium chloride solution. The separated solutions were concentrated and transfered to the alumina column for clean up, and eluated with 1-chlorobutane : methanol solution. As a results their recovering for 0.200 and 1.00ppm muarimol spiked on apples have shown 79~95%. Residual amounts of nuarimol in apple was 0.0830ppm when the fungicide was treated eight times until 3 days before its harvest. It seems to be safely used when nuarimol is treated six times until 7 days before harvest of apple.

• Journal of Food Hygiene and Safety
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• v.1 no.2
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• pp.171-176
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• 1986

ABSTRACT-In order to detect the aflatoxins in home-made Takju and peanut butter, the samples were collected in Chungbuk region and cleaned up Sep-pak silica cartridge. Aflatoxins were detected by thin layer chromatographic and high performance liquid chromatographic behavior. Determination was carried out by thin layer densitometer. The results were as follows; 1. Aflatoxin B, was detected in 78% of the home-made Takju, and the highest concentration was 1.2 ppb and average 0.36 ppb. 2. Aflatoxins were not detected in any peanut butter smaples. 3. Clean-up method by Sep-pak silica cartridge was more efficient and economical than column chromatography of AOAC method.method.

• Journal of Food Hygiene and Safety
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• v.18 no.2
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• pp.43-50
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• 2003

A liquid chromatographic method, using matrix solid-phase dispersion (MSPD) is developed for the extraction of residual furazolidone in chicken eggs. Blank or fortified egg samples (0.5 g) were blended with Octadecylsilyl (Bulk $C_{18}$, 40${\mu}{\textrm}{m}$, 18%. load, endcapped. 2 g) derivatized silica. After homogenization, $C_{18}$/egg and Na$_2$S $O_4$matrix were transferred to a column made of 10 ml glass syringe and filter paper and compressed 4.0∼4.5 ml volume. The column was washed with 8 ml of hexane and dried under $N_2$ gas. Furazolidone was eluted with acetonitrile (8 ml) under gravity. The eluate containing furazolidone was free from interfering compounds when analyzed by HPLC with UV detection (365 nm, photodiode array). Calibration curves were linear (r = 0.99985) and inter- (1.47%) and intra-assay (5.29%) variabilities for the concentration range examined (7.8∼497 ng/g of eggs, 20 ${mu}ell$ injection volume) were indicative of an acceptable methodology for the analysis of furazolidone. Average recovery of furazolidone added to egg was 96.2%. The limit of detection for the proposed method was 1 ng/g for furazolidone. The method using MSPD is proposed as an alternative assay to the classical method which involves the use of large volumes of a harmful solvent and requires a long tedious separation and clean-up processes prior to its determination.

• Journal of Korean Society on Water Environment
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• v.21 no.3
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• pp.219-229
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• 2005

The analytical methods for dioxins in water sample from wastewater to tap water were reviewed. For extraction method, liquid-liquid extraction (LLE) has been widely used, however, this process needs too much time and man power. New approach including solid phase extraction (SPE) is now applicable to large volume of water sample with high extraction efficiency. Column clean up in classical analytical methods were very complex and time consuming procedures during decade. Modifications were tried to decrease solvent and reagents volume. Moreover, use of column connection method has been demonstrated in the environmental matrices. Instrumental configurations also have been improved, in which GC/MS/MS with large volume injection approach can analyze picogram levels. Absolute sensitivities of HRMS increased compared to old versions of double focusing sector type mass spectrometers. Based on these analytical evolutions during last 10 years, we tried to optimize the analytical method for dioxins in water sample from sample extraction to instrumental analysis.

• Clean Technology
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• v.26 no.2
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• pp.102-108
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• 2020

In recent years, packed column has been widely used in separation processes, such as absorption, desorption, distillation, and extraction, in the petrochemical, fine chemistry, and environmental industries. Packed column is used as a contacting facility for gas-liquid and liquid-liquid systems filled with random packed materials in the column. Packed column has various advantages such as low pressure drop, economical efficiency, thermally sensitive liquids, easy repairing restoration, and noxious gas treatment. The performance of a packed column is highly dependent on the maintenance of good gas and liquid distribution throughout a packed bed; thus, this is an important consideration in a design of packed column. In this study, hydraulic pressure drop, hold-up as a function of liquid load, and mass transfer in the air, air/water, and air-NH₃/water systems were studied to find the geometrical characteristic for raschig super-ring experiment dry pressure drop. Based on the results, design factors and operating conditions to handle noxious gases were obtained. The dry pressure drop of the random packing raschig super-ring was linearly increased as a function of gas capacity factor with various liquid loads in the Air/Water system. This result is lower than that of 35 mm Pall-ring, which is most commonly used in the industrial field. Also, it can be found that the hydraulic pressure drop of raschig super-ring is consistently increased by gas capacity factor with various liquid loads. When gas capacity factor with various liquid loads is increased from 1.855 to 2.323 kg^-1/2 m^-1/2 S^-1, hydraulic pressure drop increases around 17%. Finally, the liquid hold-up related to packing volume, which is a parameter of specific liquid load depending on gas capacity factor, shows consistent increase by around 3.84 kg^-1/2 m^-1/2 S^-1 of the gas capacity factor. However, liquid hold-up significantly increases above it.