• Journal of Food Hygiene and Safety
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• v.35 no.2
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• pp.109-117
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• 2020

This study aimed to develop an analytical method for determination of 18 dyes in livestock and fishery products by liquid chromatograph-tandem mass spectrometry (LC-MS/MS). The developed method was validated for linearity, accuracy, limit of quantifications (LOQ) and recovery based on the CODEX guideline (CAC/GL-71). Target matrices (beef, pork, chicken, egg, milk, flatfish, eel, and shrimp) were extracted using acetonitrile (containing 1% of acetic acid) and then, purified with C₁₈ and primary secondary amine (PSA). Calibration linearity was obtained (r²>0.98) and LOQs were 0.002 mg/kg in animal products. The recoveries of dyes were ranged from 63 to 112% and relative standard deviations (RSDs, %) were less than 15%. The residues of 18 dyes were investigated in real samples (n=124) collected from retail markets in South Korea. As a result, a total of seven samples showed positive results for target analytes in fish samples. However, there was no violation according to the maximum residue limits set by the Korean Food Code. The proposed method will be used for routine analysis of dye residues in livestock and fishery products.

• Korean Journal of Environmental Agriculture
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• v.42 no.2
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• pp.139-151
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• 2023

Sulfonylurea herbicides are widely used in agriculture because they have a long residual period and high selectivity. An analytical method was developed using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique for simultaneous determination of sulfonylurea herbicide residues in agricultural products by liquid chromatography tandem mass spectrometry and for establishment MRL (Maximum Residue Limit) of those herbicides in Korea. Extraction was performed using acetonitrile containing 0.1% formic acid with MgSO₄ (anhydrous magnesium sulfate) and NaCl (sodium chloride) and the extract was cleaned up using MgSO₄ and C₁₈ (octadecyl). The matrix-matched calibration curves were composed of 7 concentration levels from 0.001 to 0.25 mg/kg and their coefficients of determination (R²) exceeded 0.99. The recoveries of three spiking levels (LOQ, 10LOQ, 50LOQ, n=5) were in the range of 71.7-114.9% with relative standard deviations of less than 20.0% for all the five agriculture products. All validation values met criteria of the European Union SANTE/11312/2021 guidelines and Food and Drug Safety Evaluation guidelines. Therefore, the proposed analytical method was accurate, effective, and sensitive for sulfonylurea herbicide residues determination in agricultural commodities.

• Journal of Ginseng Research
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• v.40 no.3
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• pp.292-299
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• 2016

Background: We previously reported that two-phase partition chromatography between ginseng water extract and soybean oil efficiently eliminated pesticide residues. However, an undesirable odor and an unpalatable taste unique to soybean oil were two major disadvantages of the method. This study was carried out to find an alternative vegetable oil that is cost effective, labor effective, and efficient without leaving an undesirable taste and smell. Methods: We employed six vegetable oils that were available at a grocery store. A 1-mL sample of the corresponding oil containing a total of 32 pesticides, representing four categories, was mixed with 10% aqueous ginseng extract (20 mL) and equivalent vegetable oil (7 mL) in Falcon tubes. The final concentration of the pesticides in the mixture (28 mL) was adjusted to approximately 2 ppm. In addition, pesticides for spiking were clustered depending on the analytical equipment (GC/HPLC), detection mode (electron capture detector/nitrogen-phosphorus detector), or retention time used. Samples were harvested and subjected to quantitative analysis of the pesticides. Results: Soybean oil demonstrated the highest efficiency in partitioning pesticide residues in the ginseng extract to the oil phase. However, canola oil gave the best result in an organoleptic test due to the lack of undesirable odor and unpalatable taste. Furthermore, the qualitative and quantitative changes of ginsenosides evaluated by TLC and HPLC, respectively, revealed no notable change before or after canola oil treatment. Conclusion: We suggest that canola oil is an excellent vehicle with respect to its organoleptic property, cost-effectiveness and efficiency of eliminating pesticide residues in ginseng extract.

• The Korean Journal of Pesticide Science
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• v.18 no.4
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• pp.336-341
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• 2014

In order to determine the residual characteristics of pesticides in fruits and their effects on human health, monitoring of pesticide residues were conducted in apples, peaches, pears, grapes and citrus from the major cultivation areas in 2010. Safeties of the pesticides detected from the fruits were evaluated using the amounts of pesticide residue detected and dietary risk index (DRI). Samples were taken from 4-5 major fruit cultivation areas and then pesticide residues in the test fruits were analyzed with a liquid chromatographymass spectrometry (LC-MS/MS). Mean residue levels of the pesticides in fruits were 0.001-0.144 mg/kg. The DRIs were 0.55 for apple, 0.066 for peach, 0.008 for pear, 0.025 for grape, and 0.37 for citrus, respectively. The results indicated that the amounts of pesticide residues in domestic fruits might be safe, considering the regulatory concerning level 1.0.

• Korean Journal of Environmental Agriculture
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• v.39 no.3
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• pp.214-221
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• 2020

BACKGROUND: The demand for pesticide registration has kept increasing for minor crop cultivation in greenhouse since Positive List System (PLS) has been launched. Thus, much study on the evaluation of pesticide residues in minor crops is required to examine the demand. In this study, we evaluated residues of acetamiprid, boscalid, imidacloprid and pyraclostrobin in the minor crop mustard green to provide the potential data for their registration. METHODS AND RESULTS: Pesticide granule formulations of acetamiprid, boscalid, imidacloprid and pyraclostrobin were incorporated into soil and applied onto field soil surface at rates of 3 kg/10a, 6 kg/10a, 3 kg/10a and 6 kg/10a, respectively. The pesticides were also applied at the two times higher than the rates to compare the residues between the application rates. Mustard green seeds were sown 1 day after pesticide application and cultivated under greenhouse conditions. LC/MS/MS analyses coupled with a modified QuEChERs method were employed for determination of the pesticides in plant samples. The method limits of quantitation (LOQ) of the pesticides were 0.01 mg/kg, and the matrix calibration curves of the pesticides showed linearity with coefficient values of determination (r²) greater than 0.995. The average recovery values of the pesticides fortified in control samples at rates of LOQ and 10LOQ ranged from approximately 77.5% to 101.2% with relative standard deviation values lower than 14%. The pesticides in the mustard green samples cultivated for 53 days after sown were determined to be lower than the LOQ level. CONCLUSION: Acetamiprid, boscalid, imidacloprid and pyraclostrobin were found at a level lower than 0.01 mg/kg in the minor crop mustard green. Thus, their residues in mustard green would not violate PLS under greenhouse conditions.

• Journal of Food Hygiene and Safety
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• v.3 no.4
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• pp.193-202
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• 1988

A pesticide monitoring study was undertaken for the strawberry and cucumber samples collected from plastic film houses and additional strawberries from supermarkets located in Seoul city in 1983 to evaluate pesticide residues in these food commodities and also to give basic informations in establishing maximum residue limits. Organophosphorus insecticides were not detected in any cucumber samples except that diazinon found with low residue levels in two strawberry samples. Fungicide procymidone and chlorothalonil were detected with considerable high frequencies in these vegetables while their residue levels were fairly low. Even the maximum residue levels. they were much lower than maximum residue limits established in these vegetables in Environment Administration. Korea. Of the strawberries from supermarkets in Seoul city, procymidone, chlorthalonil and dichlofluanid fungicides were also detected with similar detection frequencies and residue levels to those from the plas tic film houses. By washing the strawberries with tap water, the residues were removed from 38% to 95% of the total residues. Presently, it is considered that pesticide residues in strawberry and cucumber may be no harmfullevels for food commodities.

• Journal of the Korean Society of Food Science and Nutrition
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• v.27 no.3
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• pp.471-476
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• 1998

The NO3 contents and organophosphorus pesticide residues in edible part of vegetables cultivated by a conventional or an organic farming methods were determined. The NO3 contents of vegetables cultivated by the organic farming method were between 120ppm and 4,523ppm, whereas its contents of vegetables cultivated by the conventional farming method were between 89ppm and 1,575ppm. Fifty two percent of vegetables cultivated by hte organic farming method accumulated NO3 content over than 2,000ppm, whereas 82% vegetables cultivated by the conventional farming method accumulated NO3 content below than 1,000ppm. The NO3 contents of lettuce dependent on the cultivation method obviously. The NO3 contents of lettuce cultivated by a hydroponic farming method were between 4,800 and 6,500ppm, whereas those cultivated by the conventional method were between 630 and 750ppm. The organophosphorus pesticide residues in edible part of vegetables cultivated by the conventional or the organic farming methods were not detected. The NO3 contents in edible part of vegetables cultivated by the organic farming method should be considered as one of several parameters to judge a real safe vegetable to be certified by goverment.

• The Korean Journal of Food And Nutrition
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• v.26 no.4
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• pp.865-878
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• 2013

This study is being executed to investigate the pesticide residues for agricultural products on the markets in Chungbuk area from 2010 to 2012. The samples used were chard, perilla leaf, leek, spinach, crown daisy, marsh mallow, and winter grown cabbage, These were analyzed by GC/MSD and GC/ECD. Agricultural pesticide levels of spinach was 23.4%, winter grown cabbage 20.6%, chard 14.9%, marsh mallow 14.0%, perilla leaf 13.1%, leek 8.4%, and crown daisy 5.6%. Exceeds of residual pesticides were spinach, chard, leek, perilla leaf, and marsh mallow. Based on these results, a risk assessment was being conducted by used a percentage of acceptable daily intake (%ADI). The %ADI ranged from 0.00014% to 1.73910%, and these values was indicated to have no effects on human health.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.210-217
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• 2015

Ipfencarbazone is a herbicide of the tetrazolinone class, and is believed to be an inhibitor of very long chain fatty acids (VLCFAs), which control cell division in weeds. The objective of this study was to develop and validate an official analytical method for ipfencarbazone determination in agricultural products. The ipfencarbazone residues in agricultural products were extracted with acetone, partitioned with n-hexane, and then purified through silica SPE cartridge. Finally, the analyte was quantified by gas chromatograph-electron capture detector (GC-ECD) and confirmed with gas chromatograph/mass spectrometer(GC/MS). The linear range of ipfencarbazone was 0.01 to 1.0 mg/L with the coefficient of determination ($r^2$) of 0.9999. The limit of detection (LOD) and quantification (LOQ) was 0.003 and 0.01 mg/kg, respectively. In addition, average recoveries of ipfencarbazone ranged from 80.6% to 112.3% at the different concentration levels LOQ, 10LOQ and 50LOQ, while the relative standard deviation was 2.2-8.6%. All values were consistent with the criteria ranges requested in the CODEX guidelines. Furthermore, and inter-laboratory study was conducted to validate the method. This proposed method for determination of ipfencarbazone residues in agricultural products can be used as an official analytical method.

• Journal of Food Hygiene and Safety
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• v.30 no.2
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• pp.196-201
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• 2015

This study was conducted to monitor the current status of pesticide residues and to calculate the correlation between monthly price fluctuation and distribution of pesticide residues in leafy vegetables at the whole market in Gyeonggi-do from 2009 to 2013. From the result, the maximum residue limit (MRL) were frequently exceeded in 5 leafy vegetables which were 48 cases of crown daisy (5.8%), 28 cases of chard (5.1%), 28 cases of spinach (3.4%), 25 cases of perilla leaves (3.4%) and 24 cases of chamnamul (3.7%). The high rate of monthly pesticide residues exceeding MRL showed on crown daisy and chard observed in June and September, spinach in October to November and December to January, perilla leaves in July to August and January, and chamnamul in August to September. To calculate the correlation between monthly price fluctuation and distribution of pesticide residues, we performed the Pearson's correlation analysis. From the results, there were significant differences between monthly price and pesticide residues detected in chamnamul, spinach and perilla leaves (p < 0.05). There were also significant differences between monthly price and pesticide residues exceeding MRL in chamnamul and crown daisy (p < 0.05). Although the small number of leafy vegetables and short period were analyzed in this study, the consolidation monitor of pesticide residues according to the season and price will be needed to acquire the safety of agricultural products.