• Journal of Soil and Groundwater Environment
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• v.19 no.3
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• pp.111-122
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• 2014

Partitioning interwell tracer test (PITT) is a method to quantify and qualify a site contaminated with NAPLs (Non-Aqueous Phase Liquids). Analytical description of PITT assumes that the injection-pumping well pair is on the line of the ambient groundwater flow direction, but the test-well pair could frequently be off the line in a real field site, which could be an erroneous factor in analyzing PITT data. The purpose of this work is to study the influence of the angle of the test-well pair on the ambient groundwater flow direction based on the result from PITT. From the experiments, it was found that the obliqueness of the test-well pair to the ambient groundwater flow direction could affect the tracer test resulting in a decreased NAPL estimation efficiency. In case of an oblique arrangement of the test-well pair to the ambient flow direction, it was found that the injection of a chase fluid could enhance the estimation efficiency. An increase of the pumping rate could enhance the recovery rate but it cannot be said that a high pumping rate can increase the test efficiency because a high pumping rate cannot give partitioning tracers enough time to partition into NAPLs. The results have a implication that because the arrangement of the test-well pair is a controlling factor in performing and interpreting PITT in the field in addition to the known factors such as heterogeneity and the source zone architecture, flow direction should be seriously considered in arranging test-well pair.

• The Korean Journal of Pesticide Science
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• v.18 no.4
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• pp.321-329
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• 2014

This experiment was conducted to establish an analytical method for residues of amisulbrom, as recently developed an oomycete-specific fungicide showing inhibition of fungal respiration, in crops using HPLC-UVD/MS. Amisulbrom residue was extracted with acetonitrile from representative samples of five raw products which comprised apple, green pepper, kimchi cabbage, potato and hulled rice. The extract was diluted with 50 mL of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice sample, 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, amisulbrom was successfully separated from sample co-extractives and sensitively quantitated by ultraviolet absorption at 255 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery test on every crop samples fortified with amisulbrom at 3 concentration levels per crop in each triplication. Mean recoveries ranged from 85.3% to 105.6% 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 amisulbrom was 0.04 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. The proposed method was sensitive, reproducible and easy-to-operate enough to routinely determine the residue of amisulbrom in agricultural commodities.

• 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 Korean Society of Environmental Engineers
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• v.32 no.8
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• pp.747-753
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• 2010

This study was performed to investigate the removal characteristics of volatile organic compounds (VOCs) in the gasphase biofilters, and to propose a stoichiometric analysis approach to characterize biological reaction through carbon mass balance. The VOCs studied were toluene, styrene, methyl ethyl ketone (MEK), and methyl isobutyl ketone (MIBK) as a single substrate for each biofilter. The critical loading rate was determined to be $46.9\;g/m^3{\cdot}hr$, $25.8\;g/m^3{\cdot}hr$, $96.3\;g/m^3{\cdot}hr$, and $66.5\;g/m^3{\cdot}hr$ for toluene, styrene, MEK, and MIBK, respectively. The obtained results indicated that the critical loading rate was well correlated the octanol-water partition coefficient. In the analysis of carbon mass balance, carbon recovery to $CO_2$ became relatively lower as substrate loadings increased, but higher for carbon recovery to biomass. Stoichiometric analysis revealed that biomass yield increased as substrate loadings increased, and its coefficient (g biomass/g substrate) varied from 0.31 to 0.57 for toluene, 0.29 to 0.57 for styrene, 0.08 to 0.56 for MEK, and 0.14 to 0.53 for MIBK.

• 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.

• 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.17 no.2
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• pp.84-93
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• 2013

Validated analytical methods for isopyrazam are meager or lacking. In the present study, a single residual analytical method was developed for isopyrazam in selected commodities. Isopyrazam was analyzed in brown rice, soybean, green pepper, mandarin, cucumber, and Korean melon. We tried different solvents and methods through extraction, partition and purification steps to obtain best analytical results. For isopyrazam samples were extracted with acetonitrile, concentrated and partitioned with n-hexane, clean-up using florisil with n-hexane/ethylacetate (70/30) and analyzed with HPLC/UVD. The limit of quantitation (LOQ) for isopyrazam was 1.0 ng (S/N > 10) and method LOQ (MLOQ) was 0.04 mg $kg^{-1}$. Recovery ranged through 81.0~105.3% (syn-isomer) and 80.8~105.6% (anti-isomer) at fortification level of 0.04 (MLOQ), 0.4 (10 ${\times}$ MLOQ), and 2.0 (50 ${\times}$ MLOQ). The coefficient of variation (CV) for isopyrazam was less than 10% regardless of sample types. These results were further confirmed with LC/MS, respectively. The proposed method is highly reproducible and sensitive and is suitable for routine analysis.

• The Korean Journal of Pesticide Science
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• v.15 no.2
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• pp.149-159
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• 2011

Bentazone is benzothiadiazole group herbicide, and used to foliage treatment. This herbicide have already been widely used for cereals and vegetables planting in worldwide. This experiment was conducted to establish a determination method for bentazone residue in crops using HPLC-UVD/MS. Bentazone residue was extracted with acetone (adjusted pH 1 with phosphoric acid) 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 bentazone from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The bentazone was quantitated by HPLC with UVD, using a YMC ODS AM 303 ($4.6{\times}250$ mm) column. The crops were fortified with bentazone at 3 levels per crop. Mean recovery ratio were ranged from 82.0% for a 0.2 mg/kg in apple to 97.9% for a 0.02 mg/kg in Chinese cabbage. The coefficients of variation were ranged from 0.5% for a 0.02 mg/kg in soybean to 9.7% for a 0.02 mg/kg in Chinese cabbage. Quantitative limit of bentazone was 0.02 mg/kg in representative five 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 bentazone in agricultural commodities.

• The Korean Journal of Pesticide Science
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• v.15 no.2
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• pp.125-133
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• 2011

Ametryn is used in USA, China, and Japan, but not introduced in Korea yet. So, MRL (Maximum Residue Level), and analytical method of ametryn were not establishment in Korea. Therefore, this experiment was conducted to establish a determination method for ametryn residue in crops using HPLC-UVD/MS. Ametryn 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 ametryn from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The ametryn was quantitated by HPLC with UVD, using a Tosoh ODS 120T ($4.6{\times}250$ mm) column. The crops were fortified with ametryn at 2 levels per crop. Mean recovery ratio were ranged from 83.7% for a 0.2 mg/kg in soybean to 91.1% for a 1.0 mg/kg in hulled rice. The coefficients of variation were ranged from 1.2% for a 1.0 mg/kg in hulled rice to 3.6% for a 1.0 mg/kg in soybean. Quantitative limit of amatryn was 0.02 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 ametryne in agricultural commodities.

• Journal of Applied Biological Chemistry
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• v.59 no.4
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• pp.331-336
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• 2016

Analytical methods for methiozolin in soil, water and turfgrass were established and dissipation patterns of methiozolin in soil and turfgrass were elucidated. Analysis was done using a high performance liquid chromatography with an ultra violet detector at the wavelength of 280 nm after extraction with acetone, liquid-liquid partition with dichloromethane, and a solid phase extraction purification. Limit of determination and Limit of quantitation were 1.0, 0.5, 1.0 ng, and 0.001, 0.1, 0.01 mg/kg for water, turfgrass, and soil, respectively. Recovery rates of methiozolin from soil, water, and turfgrass were ranged 87.5~111.3, 92.8~97.4, and 78.2~98.5 %, respectively. The turfgrass and soil samples were collected at 0, 1, 4, 7, 14, 30, 45, and 60 after spray on green area in golf course. Residues of methiozlolin were not translocated to lower soil layer but detected only in turfgrasses and root area of turfgrass. Half-lives of methiozolin in turfgrass were 10.7 days and 8.8 days in soil from root area.