• Korean Journal of Environmental Agriculture
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• v.40 no.2
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• pp.134-141
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• 2021

BACKGROUND: The analytical method was established for determination of fungicide chinomethionat in several animal commodities using gas chromatography (GC) coupled with electron capture detector (ECD). METHODS AND RESULTS: In order to verify the applicability, the method was optimized for determining chinomethonat in various livestock products including beef, pork, chicken, milk and egg. Chinomethionat residual was extracted using acetone/dichloromethane(9/1, v/v) with magnesium sulfate and sodium chloride (salting outassociated liquid-liquid extraction). The extract was diluted by direct partitioning into dichloromethane to remove polar co-extractives in the aqueous phase. The extract was finally purified with optimized silica gel 10 g. CONCLUSION: The method limit of quantitation (MLOQ) was 0.02 mg/kg, which was in accordance with the maximum residue level (MRL) of chinomathionate as 0.05 mg/kg in livestock product. Recovery tests were carried out at two levels of concentration (MLOQ, 10 MLOQ) and resulted in good recoveries (84.8~103.0%). Reproducibilities were obtained (Coefficient of variation <5.2%), and the linearity of calibration curves were reasonable (r²>0.995) in the range of 0.01-0.2 ㎍/mL. This established analytical method was fully validated and could be useful for quantification of chinomathionat in animal commodities as official analytical method.

• The Korean Journal of Pesticide Science
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• v.20 no.3
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• pp.247-263
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• 2016

Safe animal feed is important for the health of animals, the environment and for the safety of foods of animal origin. Therefore, the aims of this study were: 1) to validate simultaneous analytical method and 2) to investigate the amount of pesticide residues in animal feed from Republic of Korea as a part of official control. A total of 126 samples were collected in 2015 and analyzed for 105 pesticides. According to pesticides monitoring result, no residue was found in 84.1% of the samples, whereas 15.9% of samples contained pesticide residues below the maximum residue limits (MRLs). Pirimiphos-methyl and cyproconazole were the two most frequently found pesticides. The results show that all commercial feed monitored in 2015 were safe under the Korean MRL and occurrence of pesticide residues in animal feed could not be considered serious threats to human and animal health. However, continuous monitoring with tighter regulation for pesticide residues in animal feed is recommended.

• 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.

• The Korean Journal of Pesticide Science
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• v.19 no.1
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• pp.5-13
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• 2015

A chromatographic method for the determination of imazapyr, a non-selective herbicide, in agricultural commodities was developed to use safety control of pesticide residue on crops, and was fully validated as an official method for residue analysis. Agricultural commodities, mandarin (fruit), hulled rice (cereal grains), pepper (vegetables), potato (potatoes) and soybean (beans) were extracted with methanol and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2.5 by 4N hydrochloric acid. Finally, they were analyzed by high performance liquid chromatography coupled to UV detector (HPLC-UVD). The developed method had the linearity in the range of test concentrations with coefficients of determination ($r^2$) more than 0.99. Recovery studies were carried out at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. Recoveries were ranged between 72.1 to 108.0%, with relative standard deviations less than 10%. A consistent recovery was determined according to the CODEX guidelines (CAC/GL40, 2003). Finally, LC/MS with selected ion monitoring was also applied to confirm the suspected residues of imazapyr in agricultural samples. This developed method for determination of imazapyr residues in agricultural commodities. can be used as an official method.

• Proceedings of the Acoustical Society of Korea Conference
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• 1998.06e
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• pp.411-414
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• 1998

음성의 음질 향상(Speech Enhancement)을 위한 여러 가지 방법 중에서 주파수 차감법(Spectral Subtraction)은 계산량이 적기 때문에 현재 실시간으로 Speech Enhancement를 할 수 있는 가장 적절한 방법이다. 그러나, 이 방법은 원래의 입력음성에 없던 새로운 잡음을 만들어내는 큰 단점이 있는데, 이를 제거하기 위해 많은 연구가 되어오고 있다. 이러한 연구의 방향은 대부분 주변프레임 또는 주변의 주파수 성분과의 평균을 통해 피크값을 무디게 해 줌으로써 새로 생긴 튀는 잡음을 감소시키는 것이다. 이런 방법은 음성자체의 정보 또한 평균이 되어버리게 하는 새로운 단점을 낳는데, 이런 현상은 무성음구간에서 특히 심각해진다. 본 논문에서는 입력음성의 LPC 분석으로 백색필터(Whitening Filter)를 구성하여 이를 통과시킨 잔류신호(Residual)를 주파수 차감하여 얻은 새로운 잔류신호를 역 필터링하여(Synthesis Filter) 개선된 음성을 얻는 방법을 제안하였다. 제안된 알고리듬은, 주파수 차감시 포만트(Formant)의 정보가 더 유지 될 수 있기 때문에 잔류잡음을 줄일 수 있다. 청취 테스트 결과 제안한 방법이 기존의 방법보다 잔류잡음을 더 줄이는 사실을 확인할 수 있었다.

• Korean Journal of Environmental Agriculture
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• v.37 no.4
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• pp.283-290
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• 2018

BACKGROUND: Pesticide residue analysis is an essential activity in order to establish the food safety of agricultural products. Analytical approaches to the food safety are required to meet internationally the guideline of Codex (Codex Alimentarius Commission, CAC/GL 40). In this study, we developed a liquid chromatograph-tandem mass spectrometer (LC-MS/MS) method to determine the herbicide clopyralid in food matrixes. METHODS AND RESULTS: Clopyralid was extracted with aqueous acetonitrile containing formic acid and the extracts were mixed in a citrate buffer consisted of magnesium sulfate anhydrous, NaCl, sodium citrate dihydrate and disodium hydrogencitrate sesquihydrate followed by centrifugation. The supernatants were filtered through a nylon membrane filter and used for the analysis of clopyralid. The method was validated by accuracy and precision experiments on the samples fortified at 3 different levels of clopyralid. LC-MS/MS in positive mode was employed to quantitatively determine clopyralid in the food samples. Matrix-matched calibration curves were inearranged from 0.001 to 0.25 mg/kg with r2 > 0.994. The limits of detection and quantification were determined to be 0.001 and 0.01 mg/kg, respectively. There covery values of clopyralid for tified at 0.01 mg/kg in the control samples ranged from approximately 82 to 106% with relative standard deviations below 2 0%. CONCLUSION: The method developed in this study meets successfully the Codex guideline for pesticide residue analysis in food samples. This, the method could be applicable to determine pesticides in foods produced domestically and internationally.

• Journal of agriculture & life science
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• v.45 no.5
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• pp.73-80
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• 2011

Fifty substances of pesticide were selected for analysis through the historical investigation of pesticides detected from environmental-friendly agricultural soil, and the environmental-friendly agricultural soils in Gyeongnam area were collected and then were accepted Anve (accelerated solvent extraction) and SPve (solid-phase extraction) as multiresidue extraction and clean up methods suitable to the soils. The pesticide residues were analyzed by using GC/vCD/NPD, HPLC/UV/FL, GC/MSD, or HPLC/MSD. 50 kinds of pesticides for the soils were an average of 95.5% from retrieval ratio of the 72 to 118% range, and the average of 3.0% for CV (%). Among 40 samples of soil, 20 components were detected from pesticide residues of 21 samples, and average amounts detected for these components were 0.035 for endosulfan, 0.043 for ethoprophos, 0.020 for chlorpyrifos, 0.023 for chlorfenapyr, 0.047 for flufenoxuron, 0.070 for fenvalerate, 0.266 for cypermethrin, 0.016 for lufenuron, 0.022 for bifenthrin, 0.025 for fenobucarb/BPMC, 0.043 for difenoconazole, 0.059 for fenarimol, 0.020 for kresoxim-methyl, 0.026 for tetraconazole, 0.039 for isoprothiolane, 0.017 for iprobenfos, 0.014 for nolrimol, 0.156 for fluquinconazole, 0.047 for tebuconazole, and 0.045 mg/kg for oxadiazon. Therefore it is infered that the establishment of pesticide residues limit for environmental-friendly agricultural soil is needed as soon as possible.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.227-234
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• 2019

An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.

• Proceedings of the Korean Society for Agricultural Machinery Conference
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• 2003.07a
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• pp.440-446
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• 2003

농산물의 품질 향상과 생산성 증대를 위해 농약의 적절한 사용이 필요하다. 그러나 농약을 적절히 사용해도 수확 농산물의 표면이나 내부에는 농약이 잔류할 가능성이 항상 있다. 농약의 과다한 잔류는 국민 보건상 커다란 문제가 될 수 있으므로 농약의 잔류량을 신속히 측정할 수 있는 분석법이 절실히 요구되고 있다(박, 2003). 살충제 Imidacloprid는 유기인계 살충제로 해충에 전신마비, 이완, 활동성 저하 등을 일으켜 박멸한다. 국내에서는 귤굴나방, 조팝나무 진딧물, 벼멸구, 굼벵이 류 등의 방제를 위해 감귤, 사과, 고추, 배, 장미, 복숭아 및 벼농사에 광범위하게 사용되고 있다(Bayer CropScience-Korea, 2002). (중략)

• Proceedings of the Korean Vacuum Society Conference
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• 2011.02a
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• pp.43-43
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• 2011

BN(Boron Nitride)은 온도와 압력 조건에 따라 안정한 상이 sp3 결합인 cubic 구조의 BN(cBN)과 sp2 결합인 hexagonal 구조의 BN(hBN or tBN)으로 나뉘는데, 이 중 cBN은 우수한 기계적, 물리적, 화학적 특성으로 인해 박막 분야에서 매우 높은 응용가능성을 지니고 있다. 하지만 cBN 박막의 합성과정에서의 필수적인 요소인 높은 압축잔류응력은 cBN을 응용분야에 적용하는데 있어 한계점으로 계속 남아 있었다. 그동안 이러한 잔류응력을 감소시키기 위해 열처리, 이온 주입, 제 3의 물질 첨가 등 다양한 관점에서 접근한 연구들이 진행되어 왔다. 본 연구에서는 cBN 합성과정에서 잔류응력을 감소시키기 위한 방법으로 수소를 첨가하였고, 그에 따른 잔류응력의 변화를 분석하고, 그 과정에서 잔류응력의 형성에 수소가 어떤 역할을 하는지 규명하고자 하였다. cBN 박막은 hBN을 target으로한 unbalanced magnetron sputtering를 사용하여, 실리콘 wafer 위에 합성하였다. 증착압력은 1.3mTorr로, 수소의 첨가량을 증가시키며 잔류응력과 cBN fraction을 관찰하였다. cBN fraction은 FTIR로 분석하였고, 잔류응력은 실리콘 strip의 in-situ 곡률측정법으로 계산하였다. cBN 박막의 조성과 구조 분석, 수소의 역할 규명을 위해 RBS 및 HRTEM을 이용하였다.