• 한국지하수토양환경학회:학술대회논문집
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• 한국지하수토양환경학회 2002년도 추계학술발표회
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• pp.81-85
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• 2002

The possibility of simultaneous analysis of 24 pesticides out of 30 residual pesticides which are subjected to test in the golf courses was examined. The utility of the simultaneous analysis of multi-residue pesticides was evaluated by recovery test through a standard addition method of pesticides in water, soil, and lawn grass. The experimental results of the recovery rates for individual pesticides are as follows : The number of pesticide of which average recovery was over 70% regardless of medium was 16 pesticides. These pesticides were composed of 8 organophosphorus pesticides(Chlorpyrifos, Chlorpyrifos-methyl, Diazinon, EPN, Fenitrothion, Phenthoate, Phosalone, and Toclofos-methyl). 4 organochlorinated pesticides(Daconil, Captan, Endosulfan, and Tetradifon), 2 pyrethroid pesticides(Fepropathrin, Lambda-cyhalothrin) and 2 other pesticides(Bromopropylate, Pendimethalin). On the other hand, in case of Dicofol, average recovery by medium was over 70% for water and lawn grass but was only 53.3% for soil. Therefore, the simultaneous analytical method applied in this experiment is not appropriate for analysis of Dicofol in soil. Furthermore, among 7 pesticides, 2 pesticides(Amitraz and Pyraclofos) showed that theirs average recovery rates deviated from criteria(70~130%) at almost all media, while 5 pesticides(Bensulide, Deltamethrin, Iprodione, Phosphamidon and Tralomethlin) were not detected from all media by selected GC detector(NPD or ECD).

• 한국환경농학회지
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• 제39권2호
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• pp.142-169
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• 2020

BACKGROUND: A new analytical method has been developed to determine 261 pesticide residues in herbal medicines. METHODS AND RESULTS: The extraction of pesticides was carried out by modified method of the Korea Food Standards Codex sample extraction and determination was performed using GC-MS/MS and LC-MS/MS. During the pre-treatment process of the test method, Solid-liquid separation was changed to centrifugation. The method was validated by the precision and accuracy results. 261 pesticides spiked at three level 20, 50, 100 ug/kg in herbal medicines. The limit of quantification of method were 4-40 ug/kg for GC-MS/MS and 2-45 ug/kg for LC-MS/MS, respectively. Among the pesticides analysed by GC-MS/MS and LC-MS/MS, 244 pesticides (94% of total number) in chinese matrimony vine and 224 pesticides (86% of total number) in korean angelica root and 231 pesticides (89% of total number) in jujube and 214 (82% of total number) in cnidium showed recoveries in the range of 70-120% with RSD⪯20%. CONCLUSION: These results indicated that GC-MS/MS and LC-MS/MS analysis with the sample extraction in this study can be applied to multi-residue analysis of pesticides in herbal medicines.

• 농약과학회지
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• 제15권2호
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• pp.140-148
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• 2011

식품의약품안전청에서 고시한 한약재 중 잔류농약 분석법에 따라 천궁 중 bifenthrin, chlorfenapyr 및 chlorpyrifos와 황기 중 acetamiprid, azoxystrobin을 분석한 결과 크로마토그램 상에 많은 간섭물질이 나타나고 회수율이 낮은 문제점이 나타났다. 이를 개선하기 위한 방법으로 액-액 분배 과정 대신 macroporous diatomaceous earth(MDE) 컬럼을 적용하고 정제 시 용출용매 조건을 최적화함으로써 회수율은 황기에서 acetamiprid 89.6~94.1%, azoxystrobin 86.8~94.4%, 천궁에서 bifenthrin 83.6~88.4%, chlorfenapyr 77.4~83.8%, chlorpyrifos 82.6~84.3%, 변이계수(CV)는 전체시료에서 0.5~1.7%로 나타나 잔류농약 분석기준인 70~120% 의 회수율과 10% 이내의 변이계수를 만족하였다. 액-액 분배 과정을 대신하여 MDE 컬럼을 적용함으로써 발암가능 물질로 분류된 methylene chloride 사용을 배제할 수 있어 분석자의 안전성을 증대시킬 수 있었다. 또한 발생하는 폐액의 감소와 전처리 시 노동력 및 시간의 절감, 분석자간의 재현성 양호 등의 이점도 얻을 수 있었다.

• 한국지하수토양환경학회지:지하수토양환경
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• 제11권4호
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• pp.18-24
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• 2006

다성분 동시분석방법의 적용성을 검토하기 위하여 골프장 농약잔류량검사 대상항목 30종 중 다성분 동시분석이 가능할 것으로 판단되는 24종(유기인계 농약 11종, 유기염소계 농약 5종, 합성피레스로이드계 농약 4종 및 기타 농약 4종 및 농약성분에 대한 토양 잔디 물 등 매체별 회수율 실험 결과, 다성분 동시분석방법의 적용이 가능한 농약은 16종이었으며, 모든 매체에서 70% 이상의 회수율을 보였다. 이들 농약을 계통별로 분류하면, 유기인계 농약 8종(chlorpyrifos, chlorpyrifos-methyl, diazinon, EPN, fenitrothion, phenthoate, phosalone, and toclofos-methyl), 유기염소계 농약 4종(daconil, captan, endosulfan, and tetradifon), 합성피레스로이드계 농약 2종(fepropathrin, lambda-cyhalothrin), 기타 농약 2종(bromopropylate, pendimethalin)이었다. 다성분 동시분석방법의 적용 할 수 없는 8종의 농약 중 dicofol의 경우는, 물과 잔디에서는 회수율이 70%를 상회하였으나, 토양에서는 53%로 나타나 토양의 경우 다성분 동시분석방법의 적용은 어려운 것으로 판단되었다. 또한 amitraz는 매체별 회수율이 70% 이하였고, pyraclofos는 매체별 평균 회수율이 다성분 동시분석방법 적용기준($70{\sim}130%$)에 벗어났으며, bensulide, deltamethrin, iprodione, phosphamidon, tralomethlin의 농약은 전혀 검출되지 않아 본 연구에서 사용한 다성분 동시분석방법을 적용할 수 없었다.

• 한국환경농학회지
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• 제30권1호
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• pp.89-97
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• 2011

축산물 중 cypermethrin 잔류를 예로 농약 및 농물용의 약품으로 사용되는 약제와 이성질체를 포함한 약제에 대한 잔류허용기준 설정의 문제점과 개선사항을 실험과 문헌을 통해 검토하였다. 과학적이고 합리적인 잔류허용기준설정을 위해서는 분석 대상 시료 및 적용부위의 명확성과 합의된 정의의 도출 그리고, 분석 대상화합물의 명확한 지정이 있어야 한다. 그리고 이를 바탕으로 규제 검사, 연구목적의 모니터링, 관련 분석법 개발 등이 보다 깊은 연관성을 가질수 있도록 관련 전문가들의 관심과 합의점 도출은 매우 중요하다.

• 생약학회지
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• 제51권3호
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• pp.207-216
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• 2020

The analysis method for qualitative analysis of the screening method that can be performed prior to the quantitative analysis of individual pesticide was reviewed in order to meet the safety standards that are being strengthened in the field of pesticide residue testing of herbal medicines. Among the residual pesticides presented in the Korean Pharmacopoeia, 56 pesticides, excluding 15 pesticides that need to be individually analyzed, were selected for analysis using QuEChERS preprocessing and GC-MS/MS, which are used in the existing agricultural products field. For each pesticide, the detection limit level of 0.001-0.005 mg/kg and the quantitative limit level of 0.002-0.017 mg/kg were confirmed. In the recovery test in which the standard was treated at a concentration of 0.02 mg/kg, it was confirmed that the proportion of pesticides satisfying the recovery of 70-120% was 85.7-96.4% for each herbal medicine, so it was confirmed that it was a level that could be reviewed by the screening method.

• 한국환경과학회지
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• 제15권1호
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• pp.85-94
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• 2006

The simultaneous analysis of multi-residual pesticides was developed using a gas chromatography (GC) method. In this study, a simple and reliable methodology was improved to detect 154 kinds of pesticides in sinseng extract sample by using a liquid-liquid extraction procedure, open column chromagraphy and chromatographic analysis by CC electron capture detector (ECD) and GC nitrogen-phosphorus detector (NPD). The 154 kinds of pesticides were classified in 4 groups according to the chemical structure. The extraction of pesticides was experimented with $70\%$ acetone and dichloromethane/petroleum ether in order, and cleaned up via open column chromatography $(3\times30cm)$ packed with florisil $(30g,\;130^{\circ}C,\;12hrs)$. The final extract was concentrated in a rotator evaporator at $40^{\circ}C$ until dryness. Then the residue was redissolved to 2ml with acetone, and analyzed by GC-ECD and GC-NPD. The applied concentration of pesticides was over $1\~10{\mu}g/ml$. The recovery tests were ranged from $70.7\%$ to $115.2\%$ with standard deviations between 0.3 and $5.7\%$ of the standard spiked to the ginseng extract sample (Group $I\~IV$). The limit of detection (LOD) ranged from 0.001 to $0.099{\mu}g/ml$ (Group $I\~IV$). The 9 kinds of pesticides were not detected. The developed method was applied satisfactory to the determination of the 154 kinds of pesticides in the ginseng extract with good reproducibility and accuracy.

• 한국식품영양과학회지
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• 제38권12호
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• pp.1779-1784
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• 2009

우리 국민의 주식이 되는 쌀(백미)과 콩류, 감귤류, 열대과 일류, 엽채류, 엽경채류, 근채류, 과채류, 버섯류에 속하는 농산물(989건)에 대해 8종의 EBI계 농약의 잔류 여부를 분석하였다. 그 결과 8건의 검체에서 농약이 검출되었고 농약 수는 5종이 검출되었다. 기준 미설정 농약은 2종이었으며, 곡류 134건 중 4건 검출로 3.0%, 채소류 471건 중 4건 검출로 0.8%의 검출율을 나타내었다. 그 외 콩류(48건), 견과종실류(72건), 과실류(197건), 버섯류(67건)에서는 전혀 검출되지 않았으며 부적합율은 0.1%로 나타났다. 국내 미등록농약인 paclobutrazole이 근대에서 잠정허용기준을 초과하는 것으로 확인되었다. 그리고 EBI계의 검출율은 0.8%로 매우 낮았으며 검출된 농약의 경우도 기준규격 이하로 안전한 수준이었다.

• 한국환경과학회:학술대회논문집
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• 한국환경과학회 1997년도 가을 학술발표회 프로그램
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• pp.37-39
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• 1997

Pesticide residues were extracted with 70% acetone and transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil and alumina-N, The final extract was analyzed by gas chromatography with electron-capture detector(GC/ECD) and nitrogen-phosphorus detector(GC/NPD). Recoveries of the 17 organochlorine pesticides were ranged from 60.8 to 84.9% and those of 15 organophosphorus pesticides, from 70.5 to 100.0%(except phosmet and azinphos-methyl). The minimum detectable levels of this analytical method were low (0.021-0.058 mg/kg).

• 한국환경과학회지
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• 제18권12호
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• pp.1369-1381
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• 2009

The simultaneous determination of residual pesticides was developed using a gas chromatography. In this study, a simple and reliable methodology was improved to detect 175 kinds of residual pesticides by a liquid-liquid extraction procedure, followed by chromatographic analysis by gas chromatography. The 175 kinds of residual pesticides was classified into 4 groups according to the chemical structure, column type, resolution and sensitivity. The soybean sample selected for recovery experiment was not detected any pesticides. The recovery rates were ranged from 70.6% to 119.7% in most pesticides. The relative standard deviation (RSD 0.3~5.6%) was lower than 5.6% in all cases. The limits of detection (LOD) was lower than the maximum residue levels established by Korean legislations. The method has been successfully applied to the analysis of approximately 130 real samples.