• 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.

• Korean Journal of Environmental Agriculture
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• v.41 no.2
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• pp.108-114
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• 2022

BACKGROUND: This study was performed to determine residual characteristics of soil-treated metalaxyl-M and dinotefuran in crown daisy and to evaluate the risks from intake of the residual pesticides in the crop. METHODS AND RESULTS: The pesticide granules were treated in soil on two levels, and the plants samples were collected 51 days after seeding. The analytes were extracted and partitioned using the QuEChERS extraction packet (MgSO₄ 4 g, NaCl 1 g). The quantitative methods for metalaxyl-M and dinotefuran were validated in linearity, accuracy, and precision. Risk assessments of the pesticides were performed using Korea national nutrition statistics 2019. CONCLUSION(S): The residual concentrations of metalaxyl-M in crown daisy were 0.09-0.10 mg/kg (for the treatment at 6 kg/10 a) and 0.17-0.19 mg/kg (12 kg/10 a), respectively. The residual concentrations of dinotefuran in the crop were 0.53-0.75 mg/kg (3 kg/10 a) and 1.17-1.26 mg/kg (6 kg/10 a). The amounts of pesticides were less than MRL (Maximum Residue Limits) according to the Korean MFDS (Ministry of Food and Drug Safety). The HI (Hazard Index) of metalaxyl-M and dinotefuran for consumers was 0.0075% and 0.2250%, respectively. For females in the age between 50-64, the major consumer group, the HIs of the pesticides were <3%. Considering the consumption of crown daisy, they are not considered to be of toxicological concern.

• Journal of Food Hygiene and Safety
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• v.37 no.4
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• pp.238-248
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• 2022

This study was conducted to evaluate the safety of 208 types of residue pesticides on 150 dried agricultural products in Ulsan. The pesticide residues were detected using GC-MS/MS, LC-MS/MS, GC/ECD, GC/NPD, and LC/PDA. The detection rate was 19.3% (29 of 150 samples), and 28 types of pesticides were detected. Two of the 29 pesticide residues exceeded the maximum residue limit (MRL). Difenoconazole was detected in Ulleungdo aster, and chlorothalonil and chlorpyrifos were detected in chili pepper leaves. In the vegetable group, the frequency of pesticide residues was found to be the highest in dried leafy vegetables, followed by dried fruiting vegetables other than cucurbit vegetables, and then dried stalk and stem vegetables. The pesticide types detected in the commercial dried agricultural products were fungicide (60%), insecticide (23.8%), and acaricide (16.3%). In the validation study, the values of limit of detection (LOD), limit of quantitation (LOQ), coefficient of determination (R²), and recovery rate were in the range of 0.0001-0.0409 mg/kg, 0.0003-0.1241 mg/kg, 0.994-0.999, and 81.58-116.79%, respectively. The ratio of estimated daily intake (EDI)/acceptable daily intake (ADI) was 0.00002-0.31395%.

• 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.

• Analytical Science and Technology
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• v.22 no.2
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• pp.128-135
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• 2009

This paper is the monitoring results of some heavy metals (lead, cadmium, arsenic, mercury) in herbal medicines and their intake rates. The monitoring of lead, cadmium, arsenic and mercury was carried out on 600 samples with 60 kinds of herbal medicines. And the transfer ratio of heavy metals in the water-boiled drinks w as calculated. The results show that lead was detected over the Maximum Residue Limits (MRL) in 10 samples (7 species). Cadmium was detected over the MRM in 69 samples (19 species). Arsenic was detected over the MRM in 3 samples (3 species). Mercury was detected over the MRM in 13 samples (10 species). We need continuously monitoring to ensure confidence and safety for these herbal medicines. In case of the water-boiled drink, average intake rates of lead, cadmium, arsenic and mercury are 9.77%, 6.72%, 26.1% and 6.79%, respectively.

• The Korean Journal of Pesticide Science
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• v.17 no.4
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• pp.307-313
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• 2013

This study was carried out to investigate the residual characteristics of fungicide azoxystrobin and difenoconazole in Prunus mume fruits, and establish pre-harvest residue limits (PHRL) based on dissipation and biological half-lives of fungicide residues. The fungicides were sprayed onto the crop at recommended dosage once and 3 times in 7 days interval, respectively. The samples were harvested at 0, 1, 2, 4, 6, 8, 10, 12 and 14 days after treatment. These residual pesticides were extracted with QuEChERS method, clean-up with $NH_2$ SPE cartridge, and residues were analyzed by HPLC/DAD and GLC/ECD, respectively. Method quantitative limits (MQL) of azoxystrobin were 0.03 mg $kg^{-1}$ and of difenoconazole were 0.006 mg $kg^{-1}$. Average recovery were $93.2{\pm}2.49%$, $85.5{\pm}1.97%$ for azoxystrobin at fortification levels at 0.3 and 1.5 mg $kg^{-1}$, and $100.8{\pm}6.74%$, $87.6{\pm}9.92%$ for difenoconazole at fortification levels at 0.06 and 0.3 mg $kg^{-1}$, respectively. The biological half-lives of azoxystrobin were 5.9 and 5.2 days at recommended dosage once and 3 times in 7 days interval, respectively. The biological half-lives of difenoconazole were 9.3 and 8.0 days at recommended dosage once and 3 times in 7 days interval, respectively. The PHRL of azoxystrobin and difenoconazole were recommended as 5.32 and 1.64 mg $kg^{-1}$ for 10 days before harvest, respectively.

• The Korean Journal of Pesticide Science
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• v.14 no.2
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• pp.95-103
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• 2010

Fomesafen is a selective herbicide, and used to control annual and perennial broad-leaf grass on soybean and fruit fields in USA and China, but not introduced in Korea yet. So, MRL (Maximum Residue Level), and analytical method of fomesafen were not establishment in Korea. Therefore, this experiment was conducted to establish a determination method for fomesafen residue in crops using HPLC-UVD/MS. Fomesafen residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, apple, green pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover fomesafen from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The fomesafen was quantitated by HPLC with UVD, using a Shiseido CAPCELL-PAK UG C18 column. The crops were fortified with fomesafen at 3 levels per crop. Mean recovery ratio were ranged from 87.5% for a 0.4 ppm in hulled rice to 102.5% for a 0.4 ppm in apple. The coefficients of variation were ranged from 0.6% for a 2.0 ppm in hulled rice to 7.7% for a 0.04 ppm in green pepper. Quantitative limit of fomesafen was 0.04 mg/kg in representative 5 crop samples. A LC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fomesafen in agricultural commodities.

• Journal of Food Hygiene and Safety
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• v.33 no.4
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• pp.296-305
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• 2018

Spiroxamine, one of fungicides, is used to control powdery mildew in various crops and black yellow sigatoka in bananas. The major strength of spiroxamine is to control powdery mildew in various crops and bananas yellow sigatoka in bananas. The compound has shown a high level of activity, good persistence and crop tolerance. Besides powdery mildew, good control of rust, net blotch and Rhynchosporium diseases been indicated in cereals, together with a complementary activity against Septoria diseases. In 2017, the maximum residue limit (MRL) of spiroxamine established in Korea. According to Ministry of ood and rug afety) regulations, spiroxamine residues defined only parent compound. Thus, a analytical method is needed to estimate the residue level of the parent compound. The objective of this study was to develop and validate analytical method for spiroxamine in representative agricultural commodities. Samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interfering substances. The analyte were quantified and confirmed liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive-ion mode using multiple reaction monitoring (MRM). Matrix matched calibration curves were linear over the calibration ranges ($0.0005{\sim}0.1{\mu}g/mL$) for the analyte in blank extract with coefficient of determination ($r^2$) > 0.99. For validation purposes, recovery studies will be carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries 70.6~104.6% with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges in the Codex guidelines (CAC/GL40, 2003) and MFDS guidelines. proposed analytical method be used as an official analytical method in the Republic of Korea.

• Investigative Magnetic Resonance Imaging
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• v.3 no.2
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• pp.154-158
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• 1999

Purpose : The purpose of this study was to find the optimum TE value for enhancing $T_2^{*}$ weighting effect and minimizing the SNR degradation and to compare the BOLD effects according to the changes of TE in 1.5T and 3.0T MRI systems. Materials and Methods : Healthy normal volunteers (eight males and two females with 24-38 years old) participated in this study. Each volunteer was asked to perform a simple finger-tapping task (sequential opposition of thumb to each of the other four fingers) with right hand with a mean frequency of about 2Hz. The stimulus was initially off for 3 images and was then alternatively switched on and off for 2 cycles of 6 images. Images were acquired on the 1.5T and 3.0T MRI with the FLASH (fast low angle shot) pulse sequence (TR : 100ms, FA : $20^{\circ}$, FOV : 230mm) that was used with 26, 36, 46, 56, 66, 76ms of TE times in 1.5T and 16, 26, 36, 46, 56, 66ms of TE in 3.0T MRI system. After the completion of scan, MR images were transferred into a PC and processed with a home-made analysis program based on the correlation coefficient method with the threshold value of 0.45. To search for the optimum TE value in fMRI, the difference between the activation and the rest by the susceptibility change for each TE was used in 1.5T and 3.0T respectively. In addition, the functional $T_2^{*}$ map was calculated to quantify susceptibility change. Results : The calculated optimum TE for fMRI was $61.89{\pm}2.68$ at 1.5T and $47.64{\pm}13.34$ at 3.0T. The maximum percentage of signal intensity change due to the susceptibility effect inactivation region was 3.36% at TE 66ms in 1.5T 10.05% at TE 46ms in 3.0T, respectively. The signal intensity change of 3.0T was about 3 times bigger than of 1.5T. The calculated optimum TE value was consistent with TE values which were obtained from the maximum signal change for each TE. Conclusion : In this study, the 3.0T MRI was clearly more sensitive, about three times bigger than the 1.5T in detecting the susceptibility due to the deoxyhemoglobin level change in the functional MR imaging. So the 3.0T fMRI I ore useful than 1.5T.

• Korean Journal of Environmental Agriculture
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• v.33 no.4
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• pp.388-394
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• 2014

BACKGROUND: Aclonifen is used as a systemic and selective herbicide to control a wide spectrum broad-leaf weeds by inhibition carotenoid biosynthesis, and then its MRLs(Maximum Residue Limits) will be determined in onion and garlic. In this study, a new official method was developed for aclonifen determination in agricultural products to routinely inspect the violation of MRL as well as to evaluate the terminal residue level. METHODS AND RESULTS: Aclonifen was extracted from crop samples with acetone and the extract was partitioned with dichloromethane and then purified by silica solid phase extraction(SPE) cartridge. The purified samples were detected GC using an ECD detector. Limits of detection(LOD) was 0.001 mg/kg and quantification(LOQ) was 0.005 mg/kg, respectively. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n=5). The recoveries were ranged from 74.3 to 95.0% with relative standard deviations(RSDs) of less than 8%. All values were consistent with the criteria ranges requested in the Codex guidelines(CAC/GL 40). CONCLUSION: The proposed analytical method was accurate, effective and sensitive for aclonifen determination and it will be used to as an official method in Korea.