• Journal of Applied Biological Chemistry
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• v.63 no.2
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• pp.153-159
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• 2020

The analytical method was established for simultaneous determination of fungicide prochloraz and its metabolites in several animal commodities using gas chromatography (GC) coupled with electron capture detector (ECD). Samples including beef meat, pork meat, chicken meat, milk, and egg were hydrolyzed with pyridine hydrochloride which converts prochloraz and its metabolites to 2,4,6-trichlorophenol (2,4,6-TCP) because residue definition for prochloraz was 'sum of prochloraz and its metabolites containing the 2,4,6-trichlorophenol moiety, expressed as prochloraz', for compliance with MRLs from animal commodities. Therefore, residual prochloraz was extracted with acetone, decomposed to 2,4,6-TCP, partitioned with dichloromethane, purified with aminopropyl SPE and quantified as 2,4,6-TCP with GC-ECD. The instrumental limit of quantitation and method LOQ (MLOQ) was 0.01 ㎍/mL and 0.02 mg/kg for prochloraz and 0.005 ㎍/mL and 0.01 mg/kg for 2,4,6-TCP, respectively. The linearity of the calibration curve was good with R² >0.995 in the range of 0.005-0.2 ㎍/mL. Fortification levels of prochloraz were 0.02 mg/kg (MLOQ) and 0.2 mg/kg (10MLOQ) for recovery tests. Overall recoveries of prochloraz were >90% with <10% of coefficient variation (C.V.). This established analytical method was fully validated and could be useful for quantification of prochloraz and its metabolites in animal commodities as official analytical method.

• Korean Journal of Environmental Agriculture
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• v.34 no.4
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• pp.309-317
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• 2015

BACKGROUND: An analytical method was developed using GC-ECD/MS to precisely determine the residue of fipronil, a phenylpyrazole insecticide used to control a wide range of foliar and soil-borne pests.METHOD AND RESULTS: Fipronil residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and fipronil was partitioned into n-hexane/dichloromethane (20/80, v/v) to remove polar co-extractives in the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fipronil was separated and quantitated by GC-ECD using a DB-17 capillary column. Accuracy of the proposed method was validated by the recovery from crop samples fortified with fipronil at 3 levels per crop in each triplication.CONCLUSION: Mean recoveries ranged from 86.6% to 106.0% in five representative agricultural commodities. The coefficients of variation were less than 10%. Limit of quantitation of fipronil was 0.004 mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fipronil in agricultural commodities.

• Horticultural Science & Technology
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• v.34 no.1
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• pp.183-194
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• 2016

This experiment was conducted to establish an official determination method to measure fluazinam residue in horticultural crops for import and export using GC-ECD/MS. Fluazinam residue was extracted with acetone from fresh samples of four representative horticultural products, the vegetable crops green pepper and kimchi cabbage, and the fruit crops mandarin and apple. The acetone extract was diluted with saline water and n -hexane partitioning was used to recover fluazinam from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fluazinam was separated and quantitated by GC with ECD using a DB-17 capillary column. The horticultural crops were fortified with three different concentrations of fluazinam. Mean recoveries ranged from 82.5% to 99.9% in the four crops. The coefficients of variation were less than 10.0%. The quantitative limit of fluazinam detection was $0.004mg{\cdot}kg^{-1}$ in the four crop samples. GC/MS with selected-ion monitoring was also used to confirm the suspected residue. This analytical method was reproducible and sensitive enough to measure the residue of fluazinam in horticultural commodities for import and export.

• Journal of the Korean Society of International Agriculture
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• v.30 no.4
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• pp.339-346
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• 2018

Cyanazine is a member of the triazine family of herbicides. Cyanazine is used as a pre- and post-emergence herbicide for the control of annual grasses and broadleaf weeds. This experiment was conducted to establish a determination method for cyanazine, as domestic unregistered pesticide, residue in major agricultural commodities using HPLC-DAD/MS. Cyanazine was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and partitioned to dichloromethane for remove polar extractive in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized florisil column chromatography. On a $C_{18}$ column in HPLC, cyanazine was successfully separated from co-extractives of sample, and sensitively quantitated by diode array detection at 220 nm. Accuracy and precision of the proposed method was validated by the recovery experiment on every major agricultural commodity samples fortified with cyanazine at 3 concentration levels per agricultural commodity in each triplication. Mean recoveries were ranged from 83.6 to 93.3% in five major representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation(LOQ) of cyanazine was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring(SIM) technique was also provided to clearly identify the suspected residue.

• Journal of the Korea institute for structural maintenance and inspection
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• v.17 no.6
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• pp.11-20
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• 2013

In this paper, the quantitative damage index for reinforced concrete (RC) columns with non-seismic details were presented. They are necessary to carry out the postearthquake safety evaluation of RC buildings under 5 stories without seismic details. The static cyclic test of the RC frame sub-assemblage that was an one span and actual-sized was first conducted. The specimen collapsed by the shear failure after flexural yielding of a column, lots of cracks on the surfaces of columns and beam-column joints and the cover concrete splitting at the bottom of columns occurred. The damage levels of these kinds of columns with non-seismic details were classified to five based on the load-displacement relationship by the test result. The residual story drift ratios and crack widths were then adapted as the quantitative index to evaluate the damage limit states because those values were comparatively easy to measure right after earthquakes. The highest one among the residual story drift ratios under the similar maximum story drift ratio decided on the residual story drift ratio of each damage limit state. On the other hand, the lowest and average ones among the respective residual shear and flexural widths under the similar maximum story drift ratio decided on the residual shear and flexural widths of each damage limit state, respectively. These values for each damage limit state resulted in being smaller than those by the international damage evaluation guidelines that are for seismically designed members under the same deformations.

• The Journal of Engineering Geology
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• v.18 no.3
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• pp.339-347
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• 2008

This study was carried out to assess quantitatively the safety of a tunnel by using critical strains in the ground. Critical strain is a new material property of the ground. It can be applied as deformation limits in the ground due to excavation using the measured displacement at the tunnel construction site. To achieve this purpose, the critical strain concept was reviewed and applied to assess the tunnel safety. First of all, the calculated excavation displacements of a circular tunnel by commercial programs were investigated and inputted into a feedback analysis module to calculate strains in the ground. Then the safety of tunnels was evaluated based on the critical strain concept. Subsequently the measured displacements obtained in the field are utilized practically to assess the safety of tunnels using the critical strain concept. Through this study, it was confirmed that the critical strain concept is useful to assess the safety of tunnels quantitatively.

• Journal of Food Hygiene and Safety
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• v.34 no.6
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• pp.519-525
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• 2019

The Ministry of Food and Drug Safety (MFDS) is amending its test methods for health functional foods (dietary food supplements) to establish regulatory standards and specifications in Korea. In this regard, we are continuing our research on analytical method development for the items listed in the Korean Health Functional Food Codex. In this study, we have developed a sensitive and selective test method that could simultaneously separate and determine coenzyme Q10 based on liquid chromatographic-tandem mass spectrometry (LC-MS/MS). Calibration curves showed linearity with a correlation coefficient (R²) of > 0.999 and the limits of detection (LODs) and limits of quantitation (LOQs) were in the range of 26.0 ㎍/L and 78.9 ㎍/L, respectively. The recovery results ranged between 98.6-107.0% at 3 different concentration levels with relative standard deviations (RSDs) less than 5%. The proposed analytical method was characterized with high resolution of the coenzyme Q10 and the assay was fully validated as well.

• Korean Journal of Environmental Agriculture
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• v.37 no.1
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• pp.57-65
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• 2018

BACKGROUND: An analytical method was developed using HPLC-UVD/MS to precisely determine the residue of flusulfamide, a benzenesulfonamide fungicide used to inhibit spore germination. METHODS AND RESULTS: Flusulfamide residue was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice, and soybean. The extract was diluted with large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, flusulfamide was successfully separated from co-extractives of sample, and sensitively quantitated by ultraviolet absorption at 280 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop sample fortified with flusulfamide at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries ranged from 82.3 to 98.2% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of flusulfamide was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue.

• 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.

• Journal of Korean Society of Environmental Engineers
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• v.37 no.2
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• pp.81-86
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• 2015

A simple analytical method to quantify formaldehyde in water at lower levels (${\mu}g/L$) was developed using a high performance liquid chromatography (HPLC) and acetylacetone as a derivative reagent. Unlike conventional methods, no extraction and/or concentration were required. The derivative reagent was added into samples and reacted for 30 minutes at $80^{\circ}C$ prior to the analysis of formaldehyde using HPLC. The method detection limit and the limit of quantification for this method were 1.6 and $5.0{\mu}g/L$, respectively. This method also achieved high precision (0.6-3.0%) and accuracy (91.6-106.3%). The recovery rates for various environmental samples ranged from 92.0 to 115.2%.