• 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.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.235-241
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• 2019

An analytical method was developed for the determination of an antibiotic fungicide, kasugamycin, in agricultural products (hulled rice, potato, soybean, mandarin and green pepper) using liquid chromatographytandem mass spectrometry (LC-MS/MS). Samples were extracted with methanol adjusted to pH 13 using 1 N sodium hydroxide, and purified with a HLB (hydrophilic lipophilic balance) cartridge. Linearity of a matrix-matched calibration curve using seven concentration levels, from 0.001 to 0.1 mg/kg, was excellent with a correlation coefficient ($R^2$) of more than 0.9998. The limits of detection (LOD) and quantification (LOQ) of instrument were 0.0005 and $0.001{\mu}g/mL$, respectively, and the LOQ of analytical method calculated as 0.01 mg/kg. The average recoveries at three spiking levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) were in the range of 71.2~95.4% with relative standard deviation of less than 12.1%. The developed method was simple and all optimized results was satisfied with the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. The present study could be served as a reference for the establishment of maximum residue limits (MRL) of kasugamycin and be used as basic data for safety management relative to kasugamycin residues in imported and domestic agricultural products.

• 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.

• Journal of Food Hygiene and Safety
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• v.36 no.3
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• pp.228-238
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• 2021

The aim of this research was to develop a rapid and easy multi-residue method for determining dimethipin, omethoate, dimethipin, chlorfenvinphos and azinphos-methyl in agricultural products (hulled rice, potato, soybean, mandarin and green pepper). Samples were prepared using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and analyzed using gas chromatography-tandem mass spectrometry (GC-MS/MS). Residual pesticides were extracted with 1% acetic acid in acetonitrile followed by addition of anhydrous magnesium sulfate (MgSO₄) and anhydrous sodium acetate. The extracts were cleaned up using MgSO₄, primary secondary amine (PSA) and octadecyl (C₁₈). The linearity of the calibration curves, which waas excellent by matrix-matched standards, ranged from 0.005 mg/kg to 0.3 mg/kg and yielded the coefficients of determination (R²) ≥ 0.9934 for all analytes. Average recoveries spiked at three levels (0.01, 0.1, 0.5 mg/kg) and were in the range of 74.2-119.3%, while standard deviation values were less than 14.6%, which is below the Codex guideline (CODEX CAC/GL 40).

• Journal of Food Hygiene and Safety
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• v.38 no.3
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• pp.79-88
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• 2023

Trifludimoxazin is a triazinone herbicide that inhibits the synthesis of protoporphyrinogen oxidase (PPO). The lack of PPO damages the cell membranes, leading to plant cell death. An official analytical method for the safety management of trifludimoxazin is necessary because it is a newly registered herbicide in Korea. Therefore, this study aimed to develop a residual analysis method to detect trifludimoxazin in five representative agricultural products. The EN method was established as the final extraction method by comparing the recovery test and matrix effect with those of the QuEChERS method. Various sorbent agents were used to establish the clean-up method, and no differences were observed among them. MgSO₄ and PSA were selected as the final clean-up conditions. We used LC-MS/MS considering the selectivity and sensitivity of the target pesticide and analyzed the samples in the MRM mode. The recovery test results using the established analysis method and inter-laboratory validation showed a valid range of 73.5-100.7%, with a relative standard deviation and coefficient of variation less than 12.6% and 14.5%, respectively. Therefore, the presence of trifludimoxazin can be analyzed using a modified QuEChERS method, which is widely available in Korea to ensure the safety of residual insecticides.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2006.11a
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• pp.95-96
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• 2006

CMOS Image Sensor(CIS) 소자에서 광감도의 향상과 천연색 형성을 위하여 적용하고 있는 Color-Filter 공정에서 국부적으로 발생하는 strip성 불량과 막질손상을 제거하기 위한 연구를 진행하였다. 우선 지역적 경향성을 보이는 불량에 대해서는 PR strip process type을 액조 진행방식에서 회전식으로 변경했을 때 제거됨을 확인하였고, 막질손상을 최소화하기 위해서는 새로운 유기용매의 적용이 필요하였다. 실험 결과, 케톤기를 가지는 화합물과 Polar Apotic 용매의 혼합화합물을 적용하였을 때 각 막질에 attack을 최소화하면서 원하는 PR만 선택적으로 제거 되며 미세잔류성분에 대한 제거력도 향상됨을 확인하였다.

• Analytical Science and Technology
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• v.15 no.5
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• pp.466-474
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• 2002

The analytical method of 14 kinds of coplanar - PCBs was established and applied the soil sample. The three kinds of extraction solvents (toluene, acetone: n-hexane, dichloromethane) were selected to apply the soil sample. The silica gel, florisil and alumina column cleanup also performed to compare the elution recovery. The average recovery of selected solvents in soil A, B and C was surveyed the 84.25%, 56.09% and 44.69% for toluene, 52.56%, 81.42% and 58.53% for acetone : n - hexane and 55.94%, 71.33% and 61.05% for dichloromethane. The average recovery is represented 49.99% for silica gel (n - hexane 100 mL), 69.65% for florisil (6% ether/n - hexane 100 mL), and 65.23% for alumina (2% DCM : n - hexane 100 mL, 50% DCM: n-hexane 150 mL). In silica gel (n - hexane) and florisil (6% ether : n - hexane) cleanup, the 14 kinds of coplanar PCBs eluted until 40 mL. In the silica gel and florisil columns cleanup, the amounts of elution solvent can be reduced from these results, but the researcher has to confirm the elution amounts before performing the experiments. In alumina cleanup process, the result was obtained to the 100 mL of elution solvents (2% DCM: n-hexane 100 mL and 50% DCM: n-hexane 40 mL), therefore the change of elution solvent is necessary to develop the simple procedure.

• Journal of the Korean Chemical Society
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• v.30 no.5
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• pp.465-474
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• 1986

The solvent extraction and cleanup processes for the simultaneous gas-liquid chromatographic determination of 11 kinds of organophosphorous pesticide residues in crops were investigated. The extracts dissolved with acetone were partitioned with petroleum ether after adding saturated NaCl solution. Evaporated the partitioning solvent, the residue was dissolved in methylene chloride and eluted through mixed adsorbent (1 : 2 : 4 of activated carbon, magnesia and diatomaceous earth) with methylene chloride as an eluent. The pesticides recovered were 82∼105% and the impurities were effectively removed.

• Transactions of the Korean hydrogen and new energy society
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• v.26 no.6
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• pp.547-553
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• 2015

For commercialization of fuel cell electric vehicles, one of the key objectives is to reduce cost of full stack assembly. Regarding Membrane Electrode Assembly, the major issue is to improve fuel cell activation process in the initial Hydrogen Oxidation Reaction and Oxygen Reduction Reaction. In this research, the VD (Vacuum Drying) process has been developed for improvement of activation process. The VD condition is developed by controlling the temperature and degree of vacuum to remove the remaining solvent of electrode. Consequently, the electrode applied to VD process showed the low characteristics such as 3.5% of remaining solvent content and the improved efficiency such as 15% of activation process speed.

• Analytical Science and Technology
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• v.15 no.1
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• pp.67-71
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• 2002

The residual analysis and half-life time of imidazole fungicide prochloraz in soils (silty clay) were investigated by gas chromatography equipped electron capture detector (GC-ECD). The soil samples were extracted acetone/hexane(1:1) solvent and analyzed after separated by $LC-NH_2$ Sep-Pak solid column. Linear sensitivity of standard calibration curve was Y = 268.8600X + 0.0664, $R^2=0.9998$ between 0.05~1.00 ng. The detection limit was 0.02 mg/L and the average recoveries were 94.5~97.3% from the standard additional experiments with 0.10 and 0.40 mg/L. The half-life time was 24.4 days in room laboratory and 7.6 days in the field test soil.