• Journal of Food Hygiene and Safety
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• v.32 no.4
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• pp.290-297
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• 2017

The purpose of this study was developed for the determination of tridemorph in agricultural commodities samples. Tridemorph residues in samples were extracted with acetonitrile, partitioned with saline water, and then purified using and aminopropyl ($NH_2$) SPE catridge. The purified samples were quantified and confirmed via 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 (0.005~2.5 ng) into a blank extract with $r^2$ > 0.999. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. The average recovery ranged between 75.9% and 103.7% at different concentration levels (LOQ, 10 LOQ, 50 LOQ, n = 5) with relative standard deviations (RSDs) less than 9.0%. An interlaboratory study was conducted to validate the method by Korea Advanced Food Research Institute. The average recovery ranged between 87.0% and 109.2% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n = 5) with relative standard deviations (RSDs) less than 8.0%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003) and Food Safety Evaluation Department guidelines (2016). The results prove that the developed analytical methods is accurate, effective and sensitive for tridemorph determination.

• Analytical Science and Technology
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• v.27 no.5
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• pp.234-242
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• 2014

Imicyafos which is a nematicide for controlling root-knot nematodes has been registered in the Republic of Korea in 2012, and the maximum residue limits of imicyafos are set to watermelon and korean melon as each 0.05 mg/kg. Extremely reliable and sensitive analytical method is required for ensuring food safety on imicyafos residues in agricultural commodities. Imicyafos residues in samples were extracted with acetone, partitioned with hexane and dichloromethane, and then purified with florisil. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. Linear range was between 0.1~5 mg/kg with the correlation coefficient ($r^2$) 0.99997. Average recoveries of imicyafos ranged from 77.0 to 115.4% at the spiked levels of 0.02 and 0.05 mg/kg with the relative standard deviations of 2.2~9.6%. Limit of detection and quantification were 0.005 and 0.02 mg/kg, respectively. An inter-laboratory study was conducted to validate the determination method in depth, and the results were satisfactory. All of the validation results revealed that the developed analytical method in this study is relevant for imicyafos determination in agricultural commodities and will be used as an official analytical method.

• Korean Journal of Food Science and Technology
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• v.45 no.1
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• pp.25-33
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• 2013

Clenbuterol and ractopamine, which are ${\beta}$-agonists, have been misused as a growth promoting agent in meat producing animals. Clenbuterol was banned for veterinary drug in Korea because of its problems regarding safety. Due to their adverse effects, such as cardiovascular and central nervous diseases on human health proper control and monitoring should be conducted. The existing analytical method of clenbuterol and ractopamine in the Food code was improved through our present study. The bovine muscle samples were subjected to enzymatic hydrolysis, extracted with ethyl acetate and defatted by hexane-methanol partitioning. A molecular imprinted polymer (MIP) solid phase extraction cartridge was used for clean-up and LC-MS/MS was operated in positive multiple reaction monitoring (MRM). Clenbuterol-$d_9$ and ractopamine-$d_3$ were used as an internal standard. The renewed method was validated according to the CODEX guideline. The limits of quantitation for clenbuterol and ractopamine were 0.2 and 0.5 ${\mu}g/kg$, respectively. The mean recoveries ranged in 104.2-113.5% for clenbuterol and in 107.6-118.1% for ractopamine. The improved method was able to save both time and expenses.

• Korean Journal of Environmental Agriculture
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• v.37 no.4
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• pp.283-290
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• 2018

BACKGROUND: Pesticide residue analysis is an essential activity in order to establish the food safety of agricultural products. Analytical approaches to the food safety are required to meet internationally the guideline of Codex (Codex Alimentarius Commission, CAC/GL 40). In this study, we developed a liquid chromatograph-tandem mass spectrometer (LC-MS/MS) method to determine the herbicide clopyralid in food matrixes. METHODS AND RESULTS: Clopyralid was extracted with aqueous acetonitrile containing formic acid and the extracts were mixed in a citrate buffer consisted of magnesium sulfate anhydrous, NaCl, sodium citrate dihydrate and disodium hydrogencitrate sesquihydrate followed by centrifugation. The supernatants were filtered through a nylon membrane filter and used for the analysis of clopyralid. The method was validated by accuracy and precision experiments on the samples fortified at 3 different levels of clopyralid. LC-MS/MS in positive mode was employed to quantitatively determine clopyralid in the food samples. Matrix-matched calibration curves were inearranged from 0.001 to 0.25 mg/kg with r2 > 0.994. The limits of detection and quantification were determined to be 0.001 and 0.01 mg/kg, respectively. There covery values of clopyralid for tified at 0.01 mg/kg in the control samples ranged from approximately 82 to 106% with relative standard deviations below 2 0%. CONCLUSION: The method developed in this study meets successfully the Codex guideline for pesticide residue analysis in food samples. This, the method could be applicable to determine pesticides in foods produced domestically and internationally.

• Korean Journal of Environmental Agriculture
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• v.32 no.3
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• pp.214-223
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• 2013

BACKGROUND: This study focused on the development of an analytical method about dichlorprop (DCPP; 2-(2,4-dichlorophenoxy)propionic acid) which is a plant growth regulator, a synthetic auxin for agricultural commodities. DCPP prevents falling of fruits during their growth periods. However, the overdose of DCPP caused the unwanted maturing time and reduce the safe storage period. If we take fruits with exceeding maximum residue limits, it could be harmful. Therefore, this study presented the analytical method of DCPP in agricultural commodities for the nation-wide pesticide residues monitoring program of the Ministry of Food and Drug Safety. METHODS AND RESULTS: We adopted the analytical method for DCPP in agricultural commodities by gas chromatograph in cooperated with Electron Capture Detector(ECD). Sample extraction and purification by ion-associated partition method were applied, then quantitation was done by GC/ECD with DB-17, a moderate polarity column under the temperature-rising condition with nitrogen as a carrier gas and split-less mode. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.9998, analysed from 0.1 to 2.0 mg/L concentration. Limit of quantitation in agricultural commodities represents 0.05 mg/kg, and average recoveries ranged from 78.8 to 102.2%. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 9.5% in 0.05, 0.10, and 0.50 mg/kg. CONCLUSION(S): Our newly improved analytical method for DCPP residues in agricultural commodities was applicable to the nation-wide pesticide residues monitoring program with the acceptable level of sensitivity, repeatability and reproducibility.

• Journal of Energy Engineering
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• v.23 no.1
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• pp.90-94
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• 2014

Environmental qualification (EQ) for safety-related equipment is required to ensure that those equipment will perform their required function even under the harsh environment conditions arising from design basis accident in the nuclear power plant. As a part of EQ program, the room temperature analysis in case of a loss of Heating, Ventilation, and Air Conditioning(HVAC) system was carried out to ensure the operability of the safety-related equipment of a nuclear power plant randomly chosen among the Korean nuclear power plants. In this paper, this analysis was performed in the conservative perspective using GOTHIC code. The room temperature analysis includes selecting the rooms in which the safety related equipment are located but not supported by safety related HVAC and determining the temperature of the selected rooms. Target rooms for the analysis consist of W229/W237 (Aux. feedwater pump room), W232 (Aux. feedwater tank room) and W230 (Equipment passageway). The results showed the temperature range from $43^{\circ}C$ to $83^{\circ}C$, in 72 hours after a loss of HVAC. Those values are far below of generic EQ temperature($171^{\circ}C$). Therefore, it is satisfied with EQ requirement of temperature limits on safety related equipment.

• Journal of the Korean Society of Food Science and Nutrition
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• v.38 no.10
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• pp.1457-1465
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• 2009

This study was conducted to analyze the food safety management practices and to provide data that could be used to improve food safety management at kindergarten foodservice establishments in Daegu and Gyeongbuk province. Microbiological hazard analysis was conducted from May to July, 2008 at the four foodservice establishments. A total (20 items) of foodservice facilities, cooking utensils, and equipment were tested about total plate counts, coliforms, E. coli, Staphylococcus aureus, Salmonella spp., and Listeria monocytogenes. The microbiological detected levels were higher than the critical limits for prepreparing and cooking knives, chopping boards, working tables (both prepreparing and cooking), refrigerator (inside wall), bart, basket, and tray. E. coli, Salmonella spp., and Listeria monocytogens were not detected in any samples. However, Staphylococcus aureus were detected in rubber gloves for cooking and trench in the bottom at one foodservice establishment. In conclusion, these results suggest that a prerequisite programs guideline should be provided to improve the food safety levels at kindergarten foodservice establishments and the foodservice manager must maintain proper food safety technique for foodservice facilities, cooking utensils, and equipment at kindergarten foodservice establishments to prevent cross-contamination and spread of foodborne pathogens.

• The Korean Journal of Pesticide Science
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• v.20 no.3
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• pp.236-246
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• 2016

The aim of this study was to develop an analytical method for the determination of pyribencarb and its metabolite KIE-9749 in agricultural commodities. The experiment was performed with a range of concentrations $0.05{\sim}2.5{\mu}g/g$ in apple, green pepper, potato, hulled rice, soybean, pear, peach, grape and cucumber. Each samples were extracted with acetone and cleaned by dichloromethane/saline water partition and purified with Florisil solid phase extraction (SPE) cartridge and aminopropyl SPE cartridge. Pyribencarb and KIE-9749 were separated and quantified by HPLC/UVD at 265nm using acetonitrile and water as mobile phase. The recoveries of pyribencarb and KIE-9749 were within 78.3~108.4% and 73.9~113.7% with RSD below 12.2% and 15.0%, respectively. The limits of quantification (LOQ) were both $0.05{\mu}g/g$. LC/ESI-MS/MS was optimized for confirmation of residue identity.

• The Korean Journal of Pesticide Science
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• v.21 no.1
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• pp.62-67
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• 2017

In this study, the residue patterns of flubendiamide and pyriofenone registered in the strawberry were investigated to predict pre-harvest residue limit (PHRL). The samples were harvested at 0, 1, 2, 3, 5, 7, 10 days after treatment and the pesticide residues were analyzed by HPLC/UVD. The limit of quantification (LOQ) was $0.01mg\;kg^{-1}$ for flubendiamide and pyriofenone. The recovery levels of flubendiamide and pyriofenone were $90.9{\pm}2.2%$ and $81.9{\pm}0.8%$, $87.7{\pm}2.1%$ and $85.3{\pm}1.1%$ for spiked levels of 0.01 and $0.1mg\;kg^{-1}$, respectively. The values of biological half-lives for field 1 and field 2 were 8.1 and 7.2 days for flubendiamide, 7.0 and 6.9 days for pyriofenone. According to these results, we recommends the level of PHRL on strawberry for flubendiamide and pyriofenone as 1.87 and $3.76mg\;kg^{-1}$ at 10 days before harvest, respectively.

• Journal of the Korean Society of Marine Environment & Safety
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• v.14 no.1
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• pp.45-54
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• 2008

"Summer Deadweight Tonnage(SDWT)" is used as the criteria of the berthing capacity when establishing port entry limits under current guideline. The important factors affecting to the maximum ship size of possible berthing are mass, length and breath of the ship rather than deadweight. Therefore this guideline should be modified to ensure safety and efficient operation of berth. This study aimed to propose a rational guideline to adjust the berthing capacity. In order to decide proper berthing capacity, three berths of Port of Ulsan were selected and systematic evaluations for the safety of passage transit, berthing maneuvers, ship motions at berth and stabilities of structures were conducted. Small changes of ship size had little effect on those characteristics and little significant differences were found according to the increase of ship size at the same displacement. The evaluation results of the increasement of 50% of berthing capacity at 20,000 DWT, 25% at 40,000 DWT and 13% at 150,000 DWT were within the design criteria in which the berths were built. Therefore, if the channel width, diameter of turning circle, berth length and mooring arrangements are satisfied with the criteria, the current berth limitations should be adjusted by the displacement. as substitute for the deadweight.