• Korean Journal of Veterinary Research
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• v.60 no.4
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• pp.209-213
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• 2020

This study examined the residue of dl-methylephedrine hydrochloride (MEP) on the muscle of pigs administered orally with MEP 12 g/ton feed for seven consecutive days. Twenty healthy cross swine were administered MEP. Four treated animals were selected arbitrarily to be sacrificed at 1, 2, 3, 4, and 5 days after treatment. MEP residue concentrations in the muscle were determined by liquid chromatography coupled with tandem mass spectrometry. The drug was extracted from muscle samples using 10 mM ammonium formate in acetonitrile followed by clean-up with n-hexane. The analyte was separated on an XBridgeTM hydrophilic interaction liquid chromatography column using 10 mM ammonium formate in deionized distilled water and acetonitrile. The correlation coefficient (R2) of the calibration curve was 0.9974, and the limits of detection and quantification were 0.05 and 0.15 ㎍/kg, respectively. The recoveries at three spiking levels were 94.5-101.2%, and the relative Standard Deviations was less than 4.06%. In the MEP-treated group, MEP residues on one day post-treatment were below the maximum residue limit in the muscle. The developed method is sensitive and reliable for the detection of MEP in porcine muscle tissues. Furthermore, it exhibits low quantification limits for animal-derived food products destined for human consumption.

• Korean Journal of Environmental Agriculture
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• v.41 no.2
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• pp.95-100
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• 2022

BACKGROUND: This study was aimed to determine characteristics of residues of the soil-treated boscalid and pyraclostrobin within Hylomecon vernalis and to evaluate the risks from intake of the residual pesticides in the crop. METHODS AND RESULTS: The pesticides were treated to soils at two different concentrations, and the plant samples were collected 57 days after seeding. The samples were extracted using the QuEChERS extraction kit (MgSO₄ 4 g, NaCl 1 g). The quantitative methods for boscalid and pyraclostrobin were validated using linearity, recovery, and CV (coefficient of variation). Risk assessment of the pesticides was performed using Korea national nutrition statistics 2019. CONCLUSION(S): The residual levels of boscalid were 0.02-0.05 mg/kg (for the treatment at 6 Kg/10a) and 0.05-0.08 mg/kg (for the treatment at 12 Kg/10a), respectively. The residual concentrations of pyraclostrobin were below the LOQ. The amounts of pesticides were less than Maximum Residue Limits specified by the Korean Ministry of Food and Drug Safety. The maximum hazard indices of boscalid in chwinamul and amaranth for consumers were 0.0075% and 0.1525%, respectively, and it indicates that the risk of the pesticides from the crop is considered to be low.

• Analytical Science and Technology
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• v.25 no.6
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• pp.364-369
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• 2012

Isotianil is a novel fungicide which induces systemic acquired resistance in plants. It has excellent preventive effects as low dosages against rice blast which is one of the most serious diseases in rice. The Maximum Residue Limit (MRL) of Isotianil in republic of korea was set to 0.1 mg/kg in rice, so it is necessary to determine levels of Isotianil residues in agricultural commodities for controlling food safety. Therefore, The purpose of this study was to develop analytical method for the determination of isotiical residues in agricultural commodities using GC-NPD/MSD. Isotianil was extracted with acetonitrile from apple, chinese cabbage, hulled rice, mandarin, pepper, and soybean. The extract was diluted with saline water, and then dichloromethane partition was followed to recover this fungcide from the aqueous phase. A solid phase extraction with Florisil cartridge was additionally employed for final clean up. Isotianil was analyzed and quantitated by GC-NPD and confirmed by GC-MSD. Average recovery of Isotianil ranged from 70.0 to 103.9% in six representative agricultural commodities with relative standard deviations less than 10%, and limit of quantification (LOQ) was 0.05 mg/kg.

• The Korean Journal of Pesticide Science
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• v.16 no.2
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• pp.131-136
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• 2012

This study was carried out to elucidate residual characteristics of azoxystrobin and difenoconazole in fresh ginseng. Test pesticides were sprayed onto ginseng both in 2009 for 3-year-old ginseng and in 2010 for 4-year-old ginseng according to their pre-harvest intervals (PHIs). Limit of quantitation (LOQ) of both azoxystrobin and difenoconazole was 0.003 mg/kg. Analytical methods set up for the test pesticides were considered to be suitable for the analysis of their residues in fresh ginseng, considering that their recoveries ranged from 87.58 to 112.79%. Concentration of azoxystrobin in 3-year-old ginseng ranged from 0.004 to 0.011 mg/kg and that in 4-year-old ginseng ranged from 0.007 to 0.016 mg/kg. Amounts of difenoconazole in 3- and 4-year-old ginsengs were from 0.003 to 0.007 and from 0.007 to 0.01 mg/kg, respectively, representing no accumulation effect observed in residue amount between them.

• Journal of Applied Biological Chemistry
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• v.57 no.3
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• pp.235-242
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• 2014

The purpose of this study is the establishment of scientific processes for making food safety policies. Thus, we investigated pesticide residue level of the agricultural commodities from market, and performed risk assessment. Fifteen agricultural items are chosen based on the frequency of Korean consumption. The samples were collected from 9 cities where populations are more than one million. Total 283 active ingredients were monitoring ( total sample number =232). Single-analysis of target pesticides was for three kinds of possible growth regulators and the multicomponent analysis was for 280 kinds of pesticides, a total of 283 species were selected to perform the pesticide residues. Before monitoring the analytes, the improvements of the analytical methods were done by method validations under the CODEX analytical method development guidelines and can produce metrics that represent the international standards applied in accordance with the guidelines. In addition to residual pesticides detected during monitoring we compare the ADI to EDI values using detected result and dietary consumption data which is extracted from annual market basket survey. The 163 samples were non-detected in the total 232 samples so it means that every agricultural commodity will residual pesticides-free in 70.3%. The detected residual pesticides showed for a total of 69 cases (29.7%). Two of samples violate Korean MRL (0.9%). The ratio of EDI compared to ADI resulted in only from 0.00087 to 0.902%. In result, we can assume that all detected residual pesticides are very safe level and current policies of Korean pesticides control may be working.

• Korean Journal of Food Science and Technology
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• v.41 no.6
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• pp.722-726
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• 2009

The residue distribution ratio of pesticides among the flesh, stem and leaves of hot peppers were investigated to assure the safety of pepper powder and pepper leaves. Mixed solutions of chlorothalonil (wettable powder), kresoximmethyl (water dispersible granules) and procymidone (wettable powder) were applied once onto pepper plants in a plastic film house. After 7 days, the fruits and leaves were harvested and the fruits were divided into the flesh and stems. Pesticide residues in each pepper part were then analyzed by gas chromatography. The results showed that the concentration ratios of the chemicals in the flesh:stem and flesh:leaf ranged from 1:2-5 and 1:11-39, respectively, depending on the chemical evaluated. The observed flesh:stem ratio indicates that the pesticide content of the pepper powder product can increase by 20% if pepper stems are included in the powder product. The Korea Food and Drug Administration does not set a pesticide maximum residue level (MRL) for pepper leaves if a residue ratio in leaves over flesh is more than ten times. Results from this study support non-MRL status on the pepper leaves for the studied pesticides. Additionally, we recommend that the chlorothalonil product of a wettable powder type include the phrase "prohibition of distribution or sale for pepper leaves as food" because chlorothalonil highly resided in pepper leaves as more than twenty-four times that is a criterion level to determine an inclusion of the phrase in the label of pesticide product.

• The Korean Journal of Pesticide Science
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• v.21 no.1
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• pp.17-25
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• 2017

Dissipation pattern and biological half-lives of fungicides boscalid and pyraclostrobin were calculated on jujube. The pesticides were sprayed on jujube in two different field at the standard rate, respectively. The raw agricultural commodities were harvested at 0 (2 hr), 1, 3, 5, 7, 10 and 14 days after treatment, and analyzed by HPLC/DAD. The method limit of quantification (MLOQ) was $0.02mg\;kg^{-1}$ for boscalid and pyraclostrobin. The recovery ranged 101.8~109.3% with below 5% of CV (Coefficient of variation) for boscalid and 104.2~115.4% with below 5% of CV for pyraclostrobin. An average initial deposit at field 1 and field 2 samples were observed 0.40 and $0.48mg\;kg^{-1}$ for boscalid and, 0.76 and $0.57mg\;kg^{-1}$ for pyraclostrobin, respectively. The biological half-lives of field 1 and field 2 were 11.0 and 13.2 day for boscalid, and 6.1 and 12.7 days for pyraclostrobin.

• Korean Journal of Food Science and Technology
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• v.46 no.1
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• pp.7-12
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• 2014

A sensitive and simple analytical method to identify flutianil residues in agricultural commodities was developed and validated using gas chromatography-electron capture detection (GC-ECD) and mass spectrometry (GC-MS). The flutianil residues were extracted with acetonitrile, partitioned with dichloromethane, and then purified using a silica solid-phase extraction (SPE) cartridge. The method was validated using pepper, sweet pepper, mandarin, hulled rice, soybean, and potato spiked with 0.02 or 0.2 mg/kg flutianil. The average recovery of flutianil was 76.5-108.0% with a relative standard deviation of less than 10%. The limit of detection and limit of quantification were 0.004 and 0.02 mg/kg, respectively. The result of recoveries and relative standard deviation were in line with Codex Alimentarius Commission Guidelines (CAC/GL 40). These results show that the method developed in this study is appropriate for flutianil identification and can be used to maintain the safety of agricultural products containing flutianil residues.

• Analytical Science and Technology
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• v.22 no.4
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• pp.345-353
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• 2009

The new anti-impotency analogue was identified in food source. Detection of this analogue was accomplished through screening of food samples by liquid chromatography/photodiode array detector. The spectrum pattern of analogue compound was similar to that observed for hongdenafil which was analogue of sildenafil. This new compound was isolated and purified using the liquid-liquid extraction, thin layer chromatography, column chromatography and preparative HPLC. And then those structure were identified using analytical instruments such as HPLC/PDA, LC/MS/MS and NMR. The compound was given a name to oxohongdenafil which was replaced with acetyl oxoethylpiperazinyl residue instead of sulfonyl piperazine group of sildenafil. The regulation for the abovementioned analogue, oxohongdenafil, was established by Standard of Korean food code.

• Korean Journal of Environmental Agriculture
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• v.40 no.2
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• pp.108-117
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• 2021

BACKGROUND: Dichlobentiazox is a newly registered pesticide in Korea as a triazole fungicide and requires establishment of an official analysis method for the safety management. Therefore, the aim of this study was to determine the residual analysis method of dichlobentiazox for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods were applied to establish the extraction method, and the EN method was finally selected through the recovery test. In addition, various adsorbent agents were applied to establish the clean-up method. As a result, it was found that the recovery of the tested pesticide was reduced when using the d-SPE method with PSA and GCB, but C₁₈ showed an excellent recovery. Therefore this method was established as the final analysis method. For the analysis, LC-MS/MS was used with consideration of the selectivity and sensitivity of the target pesticide and was operated in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 70-120%, with standard deviation and coefficient of variation of less than 3.0% and 11.6%, respectively. CONCLUSION: Dichlobentiazox could be analyzed with a modified QuEChERS method, and the method determined would be widely available to ensure the safety of residual pesticides in Korea.