• Korean Journal of Food Science and Technology
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• v.47 no.3
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• pp.306-320
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• 2015

This survey was carried out in 2014 to estimate the pesticide residue levels in commercial environment-friendly agricultural products in Seoul metropolitan area. Pesticide residues in 27 commodities were examined and analyzed using LC-MS/MS, which can simultaneously detect up to 85 pesticides. A total of 441 samples were collected and analyzed. Among the detected samples, the residue levels in 1.2% of organic agricultural products and 2.2% of pesticide-free agricultural products exceeded the maximum residue limits (MRLs); hence, 1.8% of the total samples exceeded the MRLs. The safety of the detected pesticides was assessed by monitoring the acceptable daily intake level (ADI) and acceptable dietary exposure (ADE) to the pesticides via consumption of the commodities. ADI and ADE are found to be 0.07728-9.46530% and 0.00141-0.17210%, respectively, which means that the residual pesticides in the environmental-friendly agricultural products in Korea are below the safe limit and therefore, pose no potential public health risks.

• Korean Journal of Environmental Agriculture
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• v.30 no.4
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• pp.446-452
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• 2011

BACKGROUND: To investigate the dissipation patterns of 3 pesticides, azoxystrobin, difenoconazole and iprodione, on green garlic after field treatment pesticides were treated as foliar treatment by single application at recommended and double the recommended rates. METHODS AND RESULTS: Residue samples were harvested at 0, 1, 2, 5, 7 and 10 days post-treatment for azoxystrobin and 0, 1, 2, 5, 7, 10, 15 and 21 days post-treatment for difenoconazole and iprodione. After preparation the fortified samples were extracted and analyzed by gas chromotography-electron capture detector (GC-ECD) to determine the residue levels. Recoveries ranged from 87 to 109% for azoxystrobin, difenoconazole and iprodione at two different levels. The limit of Quantification (LOQ) values were 0.002 mg/kg for azoxystrobin and difenoconazole and 0.01 mg/kg for iprodione. CONCLUSION(S): Half-lives of azoxystrobin, difenoconazole and iprodione in green garlic after treatment were 1.2, 3.8 and 3.2 days at recommended and 1.4, 3.3 and 3.2 at double the recommended rate, respectively. Residue level of azoxystrobin, difenoconazole and iprodione in green garlic were below the maximum residue limits (MRLs) at 0 day, 0 day and 5 days, respectively. Therefore, these pesticide were considered that residues was satisfied to the requirement of domestic trade related to the consumer safety.

• 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.

• Journal of fish pathology
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• v.35 no.1
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• pp.93-102
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• 2022

This study performed a trichlorfon (TCF) residue and pharmacokinetic analysis with Japanese eels, Anguilla japonica, to obtain baseline data to establish the maximum residue level (MRL) of TCF in A. japonica. After dipping A. japonica in 30 ppm and 150 ppm of TCF at 28℃ and 18℃, drug residue in the body was analyzed with LC-MS/MS, and these results were further analyzed with the PK solver program to obtain the pharmacokinetic parameters of TCF in the serum, muscles, and liver. The maximum concentrations (C_max) in the serum, muscles, and liver were 25.87-357.42, 129.91-1043.73, and 40.47-375.20, respectively, and the time to maximum concentration (T_max) was 0.13-1.32h, 1.17-3.34h, and 0.14-5.40h, respectively. The terminal elimination half-life (T_1/2) was 2.13-3.92h, 5.30-10.35h, and 0.65-13.81h, respectively. In the 30 mg/L concentration group, TCF was not detected in the serum of eels 96 hours after bathing, and was below the detection limit after 336 hours in muscle and liver. On the other hand, in the 150 mg/L concentration group, TCF was not detected in the serum of eels 336 hours after bathing, but was detected in muscle and liver at 336 hours. In conclusion, the results of this study would be useful in establishing the MRL of TCF in farmed A. japonica.

• Analytical Science and Technology
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• v.21 no.6
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• pp.518-525
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• 2008

Mandipropamid is a new mandelamide-type fungicide to control foliar Oomycete pathogens in some vegetables. An analytical method was developed to determine mandipropamid residues in agricultural commodities using high-performance liquid chromatography (HPLC) and liquid chromatography/mass spectrometry (LC/MS). Mandipropamid was extracted with methanol from grape, tomato, green pepper, Chinese cabbage and potato samples. The extract was diluted with saturated sodium chloride solution and distilled water, and dichloromethane partition was followed to recover the mandipropamid from the aqueous phase. Florisil column chromatography was employed to further remove interfering co-extractives prior to HPLC analysis. Reverse-phased HPLC was successfully applied to determine mandipropamid in sample extracts with the detection at its ${\lambda}_{max}$ (223 nm). Overall recoveries of mandipropamid from fortified samples averaged $99.8{\pm}1.7$ (n=6), $89.3{\pm}5.3$ (n=6), $98.7{\pm}2.2$ (n=6), $99.7{\pm}6.8$ (n=6) and $91.1{\pm}3.1$ (n=6) for grape, tomato, green pepper, Chinese cabbage and potato, respectively. Limit of quantification of the method was 0.02~0.04 mg/kg for all samples. A LC/mass spectrometry with selected-ion monitoring was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to determine the terminal residue of mandipropamid in agricultural commodities.

• Journal of Food Hygiene and Safety
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• v.38 no.3
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• pp.89-98
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• 2023

Currently, no guidelines exist regarding the maximum residues of pesticides in edible oil which is a processed food commonly consumed in Korea. This lack of guidelines hinders the evaluation of the safety of edible oil in terms of pesticide contamination. In this study, an analysis method based on heat distillation and GC-MS/MS was established by optimizing the extraction and purification procedure for 68 pesticides. Important variables in the thermal distillation procedure included heating temperature and time, and we found the nitrogen flow rate as a mobile phase and the type of dissolving solvent were not considerably affected. The determination coefficient (R²) of the residual pesticide was 0.99 or higher, and the quantitative limit (LOQ) was 0.01-0.02 mg/L. The average recovery rate (n=5) was 66.1-120.0% and the relative standard deviation was lower than ±10% when 68 pesticides were spiked at concentrations of 0.01-0.02, 0.1, and 0.5 mg/L. In addition, the within-laboratory precision was less than ±11%, meeting the Korea Food and Drug Safety Evaluation Institute's Guidelines on Standard Procedures for Preparing Food Testing Methods (2016). Therefore, the test method developed in this study can be used as a test method for managing the safety of the residual pesticide concentration in edible oil.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.218-229
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• 2015

The proficiency testing for the residue laboratories of pesticide registration was conducted in order to improve the reliability and the ability for pesticide residue analysis. On November 2012 the testing was carried out using the soil collected and kept as the moistened state for five years, which was expected to very low residue levels of pesticides. The soil was fortified with azoxystrobin, imidacloprid and methabenzthiazuron in a manner similar to prepare soil samples for indoor soil degradation test, and then sub-samples were prepared for the distribution to participants. Some of them were randomly selected for confirm of homogeneity and to ensure the stability of samples at room temperature. Samples were consisted of two soils treated as different levels, one of which was used to the assessment and another used to confirm. In addition, provided three standard solutions, respectively concentration of 10 mg/L, and untreated soil. Forty eight institutions submitted results. The medians of results were used as the assigned values for pesticide residues. Fitness for purpose standard deviation of proficiency test was calculated by applying 20% RSD as the coefficient of variation allowed in the soil residue test. Z-score was applied for evaluation of individual pesticides, and the average of the absolute value of the Z-score for the overall assessment of pesticides. Laboratories evaluated the absolute value of the Z-score less than 2 to fit the case of azoxystrobin were 48, imidacloprid and methabenzthiazuron 46.

• The Korean Journal of Pesticide Science
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• v.17 no.2
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• pp.94-106
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• 2013

The proficiency testing for the residue laboratories of pesticide registration was conducted in order to improve the reliability and the ability for pesticide residue analysis. On October 2011 the testing was carried out using the soil collected and kept as the moistened state for five years, which is expected to very low residue levels of pesticides. The soil was fortified with chlorpyrifos, metolachlor and procymidone in a manner similar to prepare soil sample for indoor soil degradation test, and then sub-samples were prepared for the distribution to participants. Some of them were randomly selected for confirm of homogeneity and to ensure the stability of samples at room temperature. Samples were consisted of two soil treated as different levels, one of which was used to the assesment and another used to confirm. In addition, provide three standard solutions, respectively concentration of 10 mg/L, and untreated soil. Forty seven institutions submitted results. The medians of results were used as the assigned values for pesticide residues. Fitness for purpose standard deviation of proficiency test was calculated by applying 20% RSD as the coefficient of variation allowed in the soil residue test. Z-score was applied for evaluation of individual pesticides, and the average of the absolute value of the Z-score for the overall assessment of pesticides. Laboratories evaluated the absolute value of the Z-score less than 2 to fit the case of chlorpyrifos and procymidone were 44, metolachlor 40.

• The Korean Journal of Pesticide Science
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• v.12 no.2
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• pp.148-154
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• 2008

This study was carried out to investigate the residue patterns of two insecticides, lambda-cyhalothrin and deltamethrin, commonly used for lettuce, under greenhouse conditions. The pesticides were sprayed with dilution of recommended and doubled doses onto lettuce. Their detection limits were $0.001\;mg{\cdot}kg^{-1}$ and mean recoveries at the fortification levels of 0.2 and $1.0\;mg{\cdot}kg^{-1}$ were from 101.17 to 104.25 and from 99.70 to 103.77%, respectively. The pesticides were gradually decreased in lettuce with time. Biological half-lives of lambda-cyhalothrin and deltamethrin were 1.7 and 1.4 days at the recommended dose and 1.8 and 1.4 days at the doubled dose, respectively. Initial residue amounts of lambda-cyhalothrin and deltamethrin at the recommended and doubled doses exceeded their MRLs. However, the residue levels of the pesticides in the crop sampled at harvest were less than their MRLs. The ratios of the estimated daily intake (EDI) to acceptable daily intake (ADI) by intake the crop harvested 10 days after spraying were less than 1% of their ADIs.

• Journal of Food Hygiene and Safety
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• v.23 no.4
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• pp.319-323
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• 2008

Analytical method for determination of florfenicol was developed for estimate veterinary drug residue of unestablished MRLs in meat. The method was validated in correspondence with the CODEX guideline for florfenicol residue in meat. The samples mixed with sodium sulfate were extracted with ethyl acetate. After clean-up, the residue was dissolved in mobile phase and analyzed using high-performance liquid chromatography with fluorescence detector. The calibration curve showed good linearity($r^2=0.9997$) within the concentration range of $0.05{\sim}1.0\;mg/kg$. The limit of detection(LOD) and limit of quantification(LOQ) were validated at 0.012 and 0.039 mg/kg, respectively. The recoveries in fortified meat ranged from 85.6 to 95.6%($1.1{\sim}5.3%$ RSD) at the 0.05 to 0.4 spiking levels. We monitored 150 samples of meats that were purchased in Korea(Seoul, Busan, Daegu, Daejeon and Gwangju). Among tested samples, florfenicol was detected in 1 of pig at the level of 0.040 mg/kg, and below LOQ in 1 of cattle, 2 of pig and 2 of chicken. The residues of florfenicol in the tested samples were within the MRLs.