• Bulletin of Food Technology
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• v.21 no.2
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• pp.49-54
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• 2008

농산물 중 잔류농약을 보다 쉽고 효율적으로 분석 할 수 있는 다성분 동시분석 방법에 따라서 UPLC-PDA을 이용하여 기기조건에 따른 검출한계 및 정량한계를 식품별 최저 MRL과 비교하여 유효성을 알아보고 회수율을 통하여 방법의 재현성을 조사한 결과 다음과 같다. 41종의 농약에 대한 검량선은 직선성이 우수하였으며 검출한계 $0.005{\sim}0.109mg/kg$으로 나타났으며 정량한계 는 $0.018{\sim}0.363ppm$으로 나타났다. Cycloprothrin 등의 경우처럼 검출기의 감응도가 최저 MRL 기준을 초과하는 농약에 대한 보완으로는 검출감도가보다 우수한 UV 검출기 등의 병행 활용이 필요하다. 회수율에 따른 재현성은 쌀의 경우 첨가 농도 0.4 mg/kg 일때 $62.09{\sim}99.58%$로 편차범위는 $1.03{\sim}13.92%$ 얻을 수 있었다.

• Analytical Science and Technology
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• v.23 no.4
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• pp.395-404
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• 2010

A multi-residual method using gas chromatography coupled with mass spectrometry (GC/MS/ MS) was developed for the analysis of 105 pesticides. This method was tested on lemons, beans and other vegetables. The pretreatment of these pesticides was performed by liquid-liquid partition followed by cleanup with solid phase extraction cartridge (SPE Florisil), after acetonitrile extraction from matrices and sodium chloride (15 g) addition. The recovery ranged from 71.1% to 126.0% except for azinphosmethyl, famoxadone, fenamidone, flufenoxuron and triadimefon in lemons and from 72.5% to 124.5% in bean. In lemon, the limit of detection (LOD) and limit of quantification (LOQ) were 0.001~150 ng/ mL and 0.004~500 ng/mL, respectively.

• Korean Journal of Food Science and Technology
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• v.30 no.4
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• pp.721-727
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• 1998

An analytical method for simultaneous and rapid determination of organophosphorus, organochlorine, carbamate, and pyrethroid pesticides in polished rice was developed. The analysis is performed by gas chromatograph with mass selective detector (GC/MSD) in selected ion monitoring (SIM) mode. Pesticides were extracted from samples with acetone by automated Soxhlet apparatus and this extract was evaporated to dryness for the analysis. The residue was dissolved in hexane, followed by a treatment with a Sep-Pak florisil catridge. Pesticides were positively confirmed by GC/MS, retention times, and ion ratios. This analytical method allows a rapid, reliable, and a good recovery of hydrophilic pesticides. Except far captafol, captan, dichlofluanid and dichlorvos, recoveries of 42 pesticides were over 70%.

• The Korean Journal of Pesticide Science
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• v.16 no.2
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• pp.137-144
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• 2012

In order to monitor the pesticide residues in rice paddy soils and paddy waters in Korea and evaluate leachabilities to groundwater of the pesticides detected, paddy soils and paddy waters were collected twice from 40 sites of rice growing paddy fields in July and August in 2011, respectively. Pesticide residues in the samples were analyzed by multi-residue method with GC and HPLC. Five pesticides, such as butachlor, cypermethrin, iprobenfos, oxadiazon, and pendimethalin were detected from thirteen paddy soils and detection rate was about 16.3%, while no pesticide was detected in paddy water. As a results of the estimation of leachabilities for the pesticides detected using GUS (groundwater ubiquity score), their GUSs were less than 1.3, representing they have no potentials to leach into groundwater.

• The Korean Journal of Pesticide Science
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• v.16 no.4
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• pp.308-314
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• 2012

In order to monitor the residual pesticides in environment friendly agricultural commodities, fruits and fruiting vegetables. Twenty-five agricultural commodities were collected twice in May and August 2011 from nine environment friendly agricultural commodities-selling supermarkets and retail stores located in eight major cities in Korea. The number of each agricultural commodity collected, 555 samples in total, was 152 organic agricultural products, 202 pesticide-free agricultural products and 201 low-pesticide agricultural products. Pesticide residues in samples were analyzed by multiresidue method for 245 pesticides using a GC-ECD/NPD and an HPLC-DAD/FLD and the peaks suspected as pesticides were identified with a GC/MSD. As a result of pesticide residue analysis, three pesticides, bifenthrin, EPN and chlorpyrifos, were detected from four samples including apple, representing a detection rate of 0.72%. The residue levels of the four pesticide-detected samples were less than their maximum residue limits (MRLs) but one pesticide EPN detected from pear exceeded its legible criterion of one twentieth MRL. Estimated daily intakes of the pesticides detected from fruits and fruiting vegetables were less than 0.76% of their maximum permissible intake.

• Korean Journal of Environmental Agriculture
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• v.31 no.2
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• pp.157-163
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• 2012

BACKGROUND: For the safety of imported agricultural products, the study was conducted to develop the analytical method of unregistered pesticides in domestic. The analytical method of 6 pesticides, chlorthal-dimethyl, clomeprop, diflufenican, hexachlorobenzene, picolinafen, and propyzamide, for a fast multi-residue analysis were established for two different type crops, orange and brown rice by GC-ECD and confirmed by mass spectrometry. METHODS AND RESULTS: The analytical method was evaluated to limit of quantification, linearity and recoveries. The crop samples were extracted with acetonitrile and performed cleanup by liquid-liquid partition and Florisil SPE to remove co-extracted matrix. The extracted samples were analyzed by GC-ECD with good sensitivity and selectivity of the method. The limits of quantification (LOQ) range of the method with S/N ratio of 10 was 0.02~0.05 mg/kg for orange and brown rice. The linearity for targeted pesticides were $R^2$ >0.999 at the levels ranged from 0.05 to 10.0 mg/kg. The average recoveries ranged from 74.4% to 110.3% with the percentage of coefficient variation in the range 0.2~8.8% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in brown rice. And the average recoveries ranged from 77.8% to 118.4% with the percentage of coefficient variation in the range 0.2~6.6% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in orange. Final determination was by gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) to identify the targeted pesticides. CONCLUSION: As a result, this developed analytical method can be used as an official method for imported agricultural products.

• The Korean Journal of Pesticide Science
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• v.13 no.3
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• pp.127-132
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• 2009

The purpose of this study is to examine changes in the pesticides residues in pepper powder by storage conditions. Analysis of pesticide residues was performed using multiresidue analytical methods and the number of pesticides detected from 60 pepper powders was 7 pesticides such as cypermethrin, fenvalerate, kresoxim-methyl, chlorpyrifos, chlorfenapyr azoxystrobin, tebuconazole. The concentrations of cypermethrin and tebuconazole were exceeded their maximum residue limits (MRLs). The degradation patterns of pesticides at $-5^{\circ}C$ were compared to those at $20^{\circ}C$ and $4^{\circ}C$. Without reference to storage temperature, degradation rates of azoxystrobin and fenvalerate were above 80%. Degradation rate of chlorpyrifos was 47% at storage $4^{\circ}C$, $20^{\circ}C$ and 34% at storage $-5^{\circ}C$. During each storage peroid, the degradation patterns were more lower at $-5^{\circ}C$ than at $20^{\circ}C$ and $4^{\circ}C$.

• Korean Journal of Environmental Agriculture
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• v.31 no.2
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• pp.164-169
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• 2012

BACKGROUND: This study was conducted to monitor the residue of pesticides and to assess their risk in domestic agricultural products, such as fruit vegetables, tomatoes, oriental melons and root vegetables, garlic, potatoes and onions. METHODS AND RESULTS: 250 samples containing both general and environment-friendly certified agricultural products were collected from traditional markets and supermarkets in 6 cities. 132 pesticides except for herbicides were analysed using the multi-residue methods by GC/ECD, GC/NPD and HPLC/UVD. 17 kinds of pesticides were detected from 42 samples, which were 32 general, 1 organic, 4 pesticide-free and 5 low pesticide agricultural products. Among those, myclobutanil detected in 1 potato and procymidone detected in 10 oriental melons were unregistered pesticides for using in Korea. Fenbuconazole detected in 1 potato and phorate detected in 1 tomato were exceeded over the MRLs established by Korea Food and Drug Administration. CONCLUSION: Based on these results, a risk assesment was conducted using a percentage of acceptable daily intake(%ADI). %ADI ranged from 0.0064% to 4.6035%, and showed these values have no effect on human health.

• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.441-452
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• 2011

This study was carried out to survey the residual characteristics of endocrine disruptor (ED)-suspected pesticides in greenhouse soils and assess their leachabilites to groundwater. Greenhouse soils were collected from 40 sites of greenhouse in 2008 in Korea. Sixteen ED-suspected pesticides which had been using in Korea, such as alachlor, benomyl, carbaryl, cypermethrin, 2,4-D, dicofol, endosulfan, fenvalerate, malathion, mancozeb, metribuzin, metiram, methomyl, parathion, trifluralin, and vinclozolin, in the soils, were analyzed by chromatographic methods using GLC-ECD and HPLC-DAD/FLD. Limits of detection (LODs) of the test pesticides ranged from 0.0004 to 0.005 mg/kg. Recoveries of the target pesticides from soil ranged from 72.69 to 115.28%. Four pesticides including cypermethrin were detected in the range of from 0.001 to 2.019 mg/kg, representing that their detection rate from greenhouse soils was 37.5%. The highest detection rate was observed from endosulfan which was detected from 16 site soils of the total samples, indicating that endosulfan is persistent in soil because of its very low mobility and high adsorption characteristics in soil. Based on the groundwater ubiquity scores (GUSs) of the pesticides detected from greenhouse soils, most of them have little possibilities of groundwater contamination except the fungicide vinclozolin with some leaching potential because of high water solubility and very low soil adsorption property.

• The Korean Journal of Pesticide Science
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• v.8 no.3
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• pp.189-197
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• 2004

Alpine and sloped-land in Gangwondo, Korea is the most important land type for cultivation of Chinese cabbage. However, farmers in these regions have major problems with insect pests, weeds and disease. Over use or inappropriate use of agrochemicals occurs frequently. No intensive study of pesticide contamination in this area has been done. The work presented in this paper addresses this deficiency. We measured pesticide residues within soil and water samples using multiresidue analysis. Samples were collected bimonthly from April to October, 2002 at three sites with to sampling spots. At the three sites, Pyeongchang, Jeongseon and Taebaeck, pesticides most frequently detected (>30% of samples) in soil samples were endosulfan, fluazinam, diniconazole, alachlor, prothiofos and dimethomorph. The amount of pesticide residues in the soils was ranged from 0.004 to $0.412\;mg\;kg^{-1}$ in these samples. Non-registered pesticides were also detected in these samples, indicating illegal use of pesticides. No pesticide were detected in the water samples collected from those sites. The results showed that pesticide residues might be dependant on physiochemical properties of pesticides, application history and soil properties. This study provides basic data for appropriate pesticide use on alpine and sloped-land in Korea.