• The Korean Journal of Pesticide Science
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• v.19 no.1
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• pp.5-13
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• 2015

A chromatographic method for the determination of imazapyr, a non-selective herbicide, in agricultural commodities was developed to use safety control of pesticide residue on crops, and was fully validated as an official method for residue analysis. Agricultural commodities, mandarin (fruit), hulled rice (cereal grains), pepper (vegetables), potato (potatoes) and soybean (beans) were extracted with methanol and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2.5 by 4N hydrochloric acid. Finally, they were analyzed by high performance liquid chromatography coupled to UV detector (HPLC-UVD). The developed method had the linearity in the range of test concentrations with coefficients of determination ($r^2$) more than 0.99. Recovery studies were carried out at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. Recoveries were ranged between 72.1 to 108.0%, with relative standard deviations less than 10%. A consistent recovery was determined according to the CODEX guidelines (CAC/GL40, 2003). Finally, LC/MS with selected ion monitoring was also applied to confirm the suspected residues of imazapyr in agricultural samples. This developed method for determination of imazapyr residues in agricultural commodities. can be used as an official method.

• The Korean Journal of Pesticide Science
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• v.14 no.1
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• pp.16-20
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• 2010

Thiosultap, a nereistoxin analog insecticide, registered in China has been used to control selected beetles and Lepidopteran pests on rice, vegetables and fruit trees. Although domestic use of thiosultap is not permitted, it is needed to monitor this insecticide from imported crops because that has been used on crops in many foreign countries, especially China. Thiosultap in hulled rice was determined as nereistoxin derived in basic condition by GC-FPD. This method accomplished ion-associated liquid-liquid partitioning for cleanup, and limit of quantification and linearity performed by the established method were 0.05 mg $kg^{-1}$ and 0.995$(r^2)$. The recoveries performed by control hulled rice fortified with thiosultap at 0.5 and 2.5 mg $kg^{-1}$ were $96.1{\pm}7.9\sim100.8{\pm}6.1%$.

• Journal of Veterinary Science
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• v.25 no.1
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• pp.18.1-18.27
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• 2024

Mastitis is one of the most widespread infectious diseases that adversely affects the profitability of the dairy industry worldwide. Accurate diagnosis and identification of pathogens early to cull infected animals and minimize the spread of infection in herds is critical for improving treatment effects and dairy farm welfare. The major pathogens causing mastitis and pathogenesis are assessed first. The most recent and advanced strategies for detecting mastitis, including genomics and proteomics approaches, are then evaluated. Finally, the advantages and disadvantages of each technique, potential research directions, and future perspectives are reported. This review provides a theoretical basis to help veterinarians select the most sensitive, specific, and cost-effective approach for detecting bovine mastitis early.

• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.22-29
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• 2019

Validamycin A is an aminoglycoside fungicide produced by Streptomyces hygroscopicus that inhibits trehalase. The purpose of this study was to develop a method for detecting validamycin A in agricultural samples to establish MRL values for use in Korea. The validamycin A residues in samples were extracted using methanol/water (50/50, v/v) and purified with a hydrophilic-lipophilic balance (HLB) cartridges. The analyte was quantified and confirmed by 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 (0.005~0.5 ng) into a blank extract with $R^2$ > 0.99. The limits of detection and quantification were 0.005 and 0.01 mg/kg, respectively. For validation validamycin A, recovery studies were carried out three different concentration levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) with five replicates at each level. The average recovery range was from 72.5~118.3%, with relative standard deviation (RSD) less than 10.3%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the NIFDS (National Institute of Food and Drug Safety) guideline (2016). Therefore, the proposed analytical method is accurate, effective and sensitive for validamycin A determination in agricultural commodities.

• 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.

• Journal of Food Hygiene and Safety
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• v.33 no.2
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• pp.110-117
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• 2018

The aim of this study was to develop an analytical method for the quantification of diazepam residues in fishery products, using liquid and gas chromatography-tandem mass spectrometry (LC-MS/MS and GC-MS/MS). The sample utilized in the study was extracted from the fish sample (crucian carp) using 0.1% formic acid in acetonitrile. For the utilization of the purification process, the dispersive solid phase extraction (dSPE) was used for LC-MS/MS, dSPE and SPE was used for GC-MS/MS, respectively. To be sure, the standard calibration curves showed a good linearity as the noted correlation coefficients, $r^2$ was > 0.99. The average recoveries for accuracy ranged in 99.8~124% for the samples which were fortified at three different levels (0.001, 0.002 and 0.010 mg/kg). The correlation coefficient for the precision effect was measured at a range of 4.01~11.8%. The limit of detection (LOD) for the diazepam analysis was 0.0004 mg/kg, and the limit of the quantification (LOQ) was 0.001 mg/kg. The proposed analytical method was characterized with a high accuracy and acceptable sensitivity to meet the established Codex Alimentarius Commission (CAC/GL71-2009) guideline requirements. We therefore established the optimal analysis method for the determination of diazepam in the fishery products using LC-MS/MS and GC-MS/MS. It would be applicable to analyze the diazepam residues in fishery products in further studies on this subject.

• Analytical Science and Technology
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• v.28 no.4
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• pp.299-307
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• 2015

In May 2012, a safety hazard issue arose because some kiwifruit growers in New Zealand had sprayed streptomycin to prevent kiwifruit canker. Therefore, for food safety management, analytical methods to determine streptomycin residues in kiwifruits are required. We developed an analytical method to determine streptomycin residues in kiwifruit samples using liquid chromatograph tandem mass spectrometer (LC-ESI-MS/MS). Streptomycin residues in samples were extracted using 1% formic acid in methanol, centrifugation for 10 min, and subsequent supernatant filtration. Purified samples were subjected to LC-ESI-MS/MS to confirm presence of and quantify streptomycin residues. Average streptomycin recoveries (6 replicates each sample) were in the range of 94.8%-110.6% with relative standard deviations of <10%. The linearity of the concentration range of 0.01-5.0 mg/kg using a matrix-matched calibration gave R² = 0.9995. The limit of quantification (LOQ) was 0.01 mg/kg. Results showed that our analytical method is rapid, simple, and sensitive, with easy sample preparation.

• Korean Journal of Food Science and Technology
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• v.45 no.5
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• pp.531-536
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• 2013

We developed a simple, sensitive, and specific analytical method for prometryn using gas chromatography-mass spectrometry (GC-MS). Prometryn is a selective herbicide used for the control of annual grasses and broadleaf weeds in cotton and celery crops. On the basis of high specificity, sensitivity, and reproducibility, combined with simple analytical operation, we propose that our newly developed method is suitable for use as a Ministry of Food and Drug Safety (MFDS, Korea) official method in the routine analysis of individual pesticide residues. Further, the method is applicable in clams. The separation condition for GC-MS was optimized by using a DB-5MS capillary column ($30m{\times}0.25mm$, 0.25 ${\mu}m$) with helium as the carrier gas, at a flow rate of 0.9 mL/min. We achieved high linearity over the concentration range 0.02-0.5 mg/L (correlation coefficient, $r^2$ >0.998). Our method is specific and sensitive, and has a quantitation limit of 0.04 mg/kg. The average recovery in clams ranged from 84.0% to 98.0%. The reproducibility of measurements expressed as the coefficient of variation (CV%) ranged from 3.0% to 7.1%. Our analytical procedure showed high accuracy and acceptable sensitivity regarding the analytical requirements for prometryn in fishery products. Finally, we successfully applied our method to the determination of residue levels in fishery products, and showed that none of the analyzed samples contained detectable amounts of residues.

• 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.

• Journal of Food Hygiene and Safety
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• v.29 no.4
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• pp.292-298
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• 2014

Tridemorph is a systemic morpholine fungicide for crops. The objective of this study was to develop reliable and sensitive analytical method for determination of tridemorph residues in tea samples for ensuring the food safety. Tridemorph residues in samples were extracted with acetonitrile after hydration, partitioned with saline water, and then purified using an aminopropyl ($NH_2$) SPE cartridge. The purified samples were detected and quantified using LC-ESI-MS/MS. The linear detection limits for tridemorph ranged from 0.02 to $1.0mgL^{-1}$ with a correlation coefficient of 0.9999. The method was validated using tea samples spiked with tridemorph at different concentration levels (0.02 and $0.05{\mu}gmL^{-1}$). The average recovery ranged between 75.0 and 84.7% with relative standard deviations less than 10%. The LOD and LOQ were 0.01 and $0.02mgL^{-1}$, respectively. The developed method was applied successfully to the identification of tridemorph in real tea samples obtained from different sources, and tridemorph was not detected in any of the samples. The results show that the developed analytical method is accurate and suitable for tridemorph determination in tea samples.