• Journal of Environmental Science International
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• v.15 no.1
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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.

• The Korean Journal of Pesticide Science
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• v.18 no.3
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• pp.141-147
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• 2014

Fenpyroximate is acaricide of pyrazole group. This acaricide have already been permitted for herb cultivation. This experiment was conducted to establish a determination method for fenpyroximate residue in herbal medicines using HPLC-PDA and HPLC-MS/MS. Fenpyroximate residue was extracted with acetone from samples of herbal which Liquorice Root (Glycyrrhiza uralensis) and Safflower Seed (Carthamus tinctorius Linne). The extract was diluted with saturated saline water and dichloromethane liquid-liquid partition (extraction) was followed to recover fenpyroximate from the aqueous phase. Amino propyl ($NH_2$) and florisil column chromatography was additionally employed for final clean up of the extract. The fenpyroximate was quantitated by HPLC-PDA and HPLC-MS/MS. The herbals were fortified with fenpyroximate at 2 or 3 levels per crop. Mean recovery ratio were ranged from 72.0 to 106.4%. The coefficients of variation were ranged from 0.2 to 4.4. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fenpyroximate in herbal medicines.

• Korean Journal of Environmental Agriculture
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• v.39 no.3
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• pp.246-252
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• 2020

BACKGROUND: Pesticides are broadly used to control weeds and pests, and the residues remaining in crops are managed in accordance with the MRLs (maximum residue limits). Therefore, an analytical method is required to quantify the residues, and we conducted a series of analyses to select and validate the quick and simple analytical method for tolpyralate in five agricultural products using QuEChERS (quick, easy, cheap, effective, rugged and safe) method and LC-MS/MS (liquid chromatography-tandem mass spectrometry). METHODS AND RESULTS: The agricultural samples were extracted with acetonitrile followed by addition of anhydrous magnesium sulfate, sodium chloride, disodium hydrogencitrate sesquihydrate and trisodium citrate dihydrate. After shaking and centrifugation, purification was performed with d-SPE (dispersive-solid phase extraction) sorbents. To validate the optimized method, its selectivity, linearity, LOD (limit of detection), LOQ (limit of quantitation), accuracy, repeatability, and reproducibility from the inter-laboratory analyses were considered. LOQ of the analytical method was 0.01 mg/kg at five agricultural products and the linearity of matrix-matched calibration were good at seven concentration levels, from 0.0025 to 0.25 mg/L (R²≥0.9980). Mean recoveries at three spiking levels (n=5) were in the range of 85.2~112.4% with associated relative standard deviation values less than 6.2%, and the coefficient of variation between the two laboratories was also below 13%. All optimized results were validated according to the criteria ranges requested in the Codex Alimentarius Commission (CAC) and Ministry of Food and Drug Safety (MFDS) guidelines. CONCLUSION: In conclusion, we suggest that the selected and validated method could serve as a basic data for detecting tolpyralate residue in imported and domestic agricultural products.

• Korean Journal of Environmental Agriculture
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• v.37 no.1
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• pp.41-48
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• 2018

BACKGROUND: This study was performed to calculate the biological half-lives and regression coefficient of bistrifluron and cyenopyrafen dissipation in peach and to estimate the Pre-Harvest Residue Limits (PHRLs). METHODS AND RESULTS: The bistrifluron and cyenopyrafen were prepared on the basis of good agricultural practice for peach and treated with a single application. Peaches were harvested at 0, 1, 3, 5, 7, 10 and 14 days after application, prepared for analysis, and analyzed by HPLC-DAD. The limits of quantitation (LOQ) of bistifluron and cyenopyrafen were 0.02 mg/kg and 0.04 mg/kg, respectively. The recoveries of bistrifluron and cyenopyrafen were 99.5~108.7% and 88.4~98.9% at two different concentration levels. The biological half-lives of field I (Sejong) and field II (Pyeongtaek) were 6.1 and 7.0 days for bistifluron, and 6.3 and 7.0 days for cyenopyrafen, respectively. The 95% confidence intervals of dissipation rate constants of bistrifluron in peach were 0.0805~0.1457 and 0.0577~0.1417 for field I and field II, respectively, and those of cyenopyrafen were 0.0911~0.1278 and 0.0576~0.1417, respectively. CONCLUSION: Residue dissipation of bistrifluron and cyenopyrafen in peach were similar to that of correction to sample weight difference during the harvest periods. This study suggests that residue dissipation rate would be helpful to set the PHRLs that protect public health.

• Journal of the Korean Society of Food Science and Nutrition
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• v.39 no.6
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• pp.902-908
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• 2010

In 2008, we monitored residual pesticides of 15 agricultural products such as rice, corn, pea, chestnut, mandarin, lemon, onion, pineapple, lettuce, chard, sweet potato stalk, burdock, squash, sweet pepper and mushroom. Agricultural commodities were collected from markets in 22 provinces (Seoul, Busan, Incheon, Daegu, Ulsan, Daejeon, Gwangju, Wonju, Pohang, Gumi, Changwon, Gimhae, Suwon, Seongnam, Bucheon, Goyang, Yongin, Cheongju, Cheonan, Jeonju, Yeosu, and Jeju). Total 48 pesticides were analysed by multi-residue method using GC/MS/MS. We analysed 1,064 samples and 34 samples (3.20%) were detected. Sweet potatostalk, burdock, chestnuts, peas, corn, chard, squash, mushroom and onions were found to be free from pesticide residues. 6 other agricultural products did not exceed MRLs (Maximum Residue Limits) by the Korean Food Code. Chloropyrifos and fenobucarb were particularly prevalent and also they were detected over 10 times in this monitoring. Nonetheless, the exposed quantity of the 7 residual pesticides is to be considered relatively safe, compared with the acceptable daily intake (ADI) of residual pesticides.

• Archives of Pharmacal Research
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• v.21 no.4
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• pp.378-384
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• 1998

The processing pathway of G-proteins and Ras family proteins includes the isoprenylation of the cysteine residue, followed by proteolysis of three terminal residues and .alpha.-carboxyl methyl esterification of the cysteine residue. Farnesylcysteine methyltransferase (FCMT) activity is responsible for the methylation reaction which play a role in the membrane attachment of a variety of cellular proteins. Four kinds of Ras protein (c-Ha-ras, c-N-Ras, c-Ki-Ras, pan-Ras) expression were detected in adenocarcinoma of human tissue by immunohistochemical method, and hematoxylin and eosin staining. The level of Ras protein in human stomach tumor tissues was much higher than in normal and peritumoral regions of the same biopsy samples. The FCMT activities of each cellular fractions were high in mitochondrial fraction followed by microsomal fraction, whole homogenate and cytosolic fraction. The inhibitory effect on FCMT activity on stomach tumor tissue was determined after treatment with 0.25 $\mu\textrm{M}$ of S-adenosyl-$_L$-homocysteine. S-adenosyl-$_L$-homocysteine inhibited FCMT activity from 11.2% to 30.5%. These results suggested that FCMT might be involved in Ras proteins activity.

• Korean Journal of Environmental Agriculture
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• v.31 no.3
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• pp.248-254
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• 2012

BACKGROUND: In order to elucidate residual characteristics of difenoconazole and thiamethoxam by treatment to sweet persimmons for one year and to generate the data for the maximum residue limit (MRL) establishment for those pesticides in or on sweet persimmon. METHODS AND RESULTS: Systemic fungicide difenoconazole WP (10% a.i.) and systemic insecticide thiamethoxam WG (10% a.i.) were sprayed onto 12~25-years-old sweet persimmons according to its preharvest interval (PHI), respectively, and then fresh sweet persimmons were harvested at 0, 1, 3, 7, 14, 21 days after treatment from pesticide-sprayed plots at each 3 sites. The analytical methods were evaluated to limit of quantification, linearity, specificity, reproducibility and recoveries. The crop samples were extracted with acetone and performed dichloromethane partition process. The extracted samples of difenoconazole were analyzed by GC-ECD and the thiamethoxam extracted samples were analyzed by HPLC with good sensitivity and selectivity of the method. The average recoveries of difenoconazole ranged from 87.5 to 99.5% with the percentage of coefficient variation in the range 4.1~7.6% at three different spiking levels(0.02, 0.2 and 2.0 mg/kg). And the average recoveries of thiamethoxam and clothianidin ranged from 88.8 to 98.9% and 83.2 to 96.6% with the percentage of coefficient variation in the range 3.6~5.0% and 3.8~9.4% at three different spiking levels(0.02, 0.2 and 2.0 mg/kg), respectively. The residue amounts ranges of difenoconazole were 0.2~0.56 mg/kg and the residue amount was decreased below the MRL level, 1.0 mg/kg, after 1 day harvest. The residue amounts ranges of thiamethoxam were 0.08~0.28 mg/kg and the residue amount was decreased below the MRL level, 0.5 mg/kg, after 1 day harvest. And the residue amount of clothianidin was below then 0.03 mg/kg for only one test site of 14 and 28 day samples. CONCLUSION: As a result, the residual amounts of difenoconazole and thiamethoxam were not exceeded the MRL of established criteria for sweet persimmon. The biological half-lives of difenoconazole and thiamethoxam were 13.6, 19.4, 16.3 and 10.0, 15.3, 14.0 days at each three test sites, respectively.

• Asian-Australasian Journal of Animal Sciences
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• v.12 no.2
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• pp.233-243
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• 1999

Food safety or sanitation are terms broadly applicable to procedures designed to ensure that food quality is high and free of factors which may adversely affect human health. These factors include zoonotic diseases and acute and chronic effects of ingesting natural and human-made xenobiotics. Use of drugs in animal production for the treatment and control of animal diseases, to promote growth rate, and to improve feed conversion efficiency has expanded year by year, thus increasing the possibilities for occurrences in animal products of residues harmful to humans. Governmental agencies have made efforts to control or prevent residue problems. The Korean Food and Drug Administration (KFDA) is charged with the responsibility of establishing tolerances for veterinary drugs, pesticides, and mycotoxins and other non-pharmaceutical substances. The Department of Veterinary Service is responsible for establishing guidelines regarding withdrawal times of drugs, approval of drugs, their uses, and sanitation enforcement of livestock products. The authors describe the toxicological basis for the establishment of tolerance levels for xenobiotics and the pharmacokinetic basis for establishing withdrawal time for veterinary drugs. The regulatory tolerance levels of chemicals in pork and swine feed, Korean regulations on the use of feed additives, rapid residue test methods, the National Residue Program, and the Food Animal Residue Avoidance Databank are discussed. Rapid EIA methods that are under development for the screening of live animals are described These methods predict tissue residues from an examination of blood samples taken from pigs before they are slaughtered.

• Korean Journal of Food Science and Technology
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• v.38 no.3
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• pp.317-324
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• 2006

Pesticide residues were monitored in agricultural products purchased at Gyeongin and Jeolla-do provinces. Total 245 pesticides were analysed by GC-MS and LC-MS/MS, and residual pesticides were detected in 70 samples (19.7%), with spinach and chard showing high detection frequency of 35%. Fifteen samples (4.2%) exceeded Korea Maximum Residue Limits (MRLs), and 30 types of pesticides were detected in samples with azoxystrobin, procymidine, endosulfan showing considerably high frequencies in respectively 14, 13, and 13 samples. The amount of 11 pesticide including chlorpyrifos, indoxacarb among them were detected over Korea MRLs. No residual pesticides were detected in 285 (80.3%) samples, and residual pesticides levels of 55 samples (15.5%) were lower than Korea MRLs, indicating 95.8% samples were relatively safe.

• Journal of Food Hygiene and Safety
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• v.25 no.3
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• pp.226-231
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• 2010

We aimed at the monitoring medroxyprogesterone acetate (MPA) residue amount in meats and confirmed the safety of its residue in meats. Optimized condition for analytical and instrumental methods was obtained by method validation. The limit of detection (LOD) and limit of quantification (LOQ) were validated at 1.5 and 5.0 ug/kg, respectively. The calibration curve showed good linearity ($r^2$ = 0.9968) within the concentration range of 5.0~50.0 ug/kg. We selected progesterone-d9 for internal standard, The recoveries in fortified meat ranged from 67.5 to 109.56% at the 3 spiking levels. As the regulation of MPA analysis method used by LC-MS/MS on other products have established. We selected 3 species of farm stock products (cattle, pig, chicken) and purchased at the markets of seven major cities. The total 196 of meat including 46 of domestic beef, 43 of import beef, 60 of domestic pork, 12 of import pork and 35 of domestic chicken. No residue of synthetic growth hormones were detected in cattle, pig and chicken samples tested.