• Korean Journal of Environmental Agriculture
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• v.40 no.4
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• pp.353-358
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• 2021

BACKGROUND: Prochloraz has been widely used as an imidazole fungicide on fruits and vegetables in Korea. Analytical approaches to evaluate prochloraz residues in herbal medicine are required for their safety management. In this study, we developed a GC-ECD method for quantitative determination of prochloraz in Platycodi Radix. The metabolite 2,4,6-trichlorophenol (2,4,6-T) was used as a target compound to evaluate total prochloraz residues as it is categorized to a representative residue definition of prochloraz. All residues containing 2,4,6-T were converted to 2,4,6-T and subjected to GC-ECD. METHODS AND RESULTS: In order to verify the applicability, the method was optimized for determining prochloraz and it metabolite 2,4,6-T in Platycodi Radix. Prochloraz and its metabolite 2,4,6-T residuals were extracted using acetone. The extract was diluted with and partitioned directly into dichloromethane to remove polar co-extractives in the aqueous phase. The extract was decomposed to 2,4,6-T, and then the partitioned ion-associate was finally purified by optimized aminopropyl solid-phase extraction (SPE). The limits of quantitation of the method (MLOQs) were 0.04 mg/kg and 0.02 mg/kg, respectively for prochloraz and 2,4,6-T, considering the maximum residue level (MRL) of prochloraz as 0.05 mg/kg in Platycodi Radix. Recovery tests were carried out at two levels of concentration (MLOQ, 10 MLOQ) and resulted in good recoveries (82.1-89.7%). Good reproducibilities were obtained (coefficient of variation < 2.8%), and the linearities of calibration curves were reasonable (r² > 0.9986) in the range of 0.005-0.5 ㎍/mL. CONCLUSION(S): The method developed in this study was successfully validated to meet the guidelines required for quantitative determination of pesticides in herbal medicine. Thus, the method could be useful to monitor prochloraz institutionally in herbal medicine.

• Journal of Food Hygiene and Safety
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• v.28 no.1
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• pp.19-23
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• 2013

A simple and rapid method has been developed and validated for simultaneous determination of each macrolides residues (spiramycin, josamycin, tilmicosin, tylosin) in chicken muscle by high-performance liquid chromatography- photo diode array (HPLC-PDA). Chicken muscle sample have been extracted with liquid-liquid extraction process; analytes was extracted by acetonitrile, and then defatted with hexane saturated by acetonitrile. The HPLC separation was performed on a Unison UK-$C_{18}$ ($150mm{\times}3.0mm$, $3{\mu}m$) with a gradient system of 0.1% trifloroacetic acid (TFA) and 0.1% trifloroacetic acid (TFA) in acetonitrile as the mobile phase. The drugs were detected at 232 nm for spiramycin and josamycin, and 287 nm for tilmicosin and tylosin. The limits of quantification (LOQs) were between 27 and $59{\mu}g/kg$; and the intra- and inter-day precision (relative standard deviation; RSD) was between 0.9-13.2 and 2.4-13.1%, respectively in chicken muscle sample. The method may has been successfully applied for multiresidue determination of four macrolides below the maximum residue limits (MRLs) established by the European Union (EU).

• Korean Journal of Environmental Agriculture
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• v.36 no.3
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• pp.211-216
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• 2017

BACKGROUND:This study was conducted to investigate residual organochlorine pesticides (ROCPs) in agricultural soils and crops. Agricultural soil samples and crop samples were collected from 93 cities and counties. METHODS AND RESULTS: Extraction and clean-up for the quantitative analysis of ROCPs were conducted by the modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. Recovery and limit of detection (LOD) of ROCPs in agriculturalsoils and crops were 76.5-103.0 and 75.2-93.2%, 0.01-0.08 and $0.10-0.15{\mu}g/kg$, respectively. Detected ROCPs in agricultural soils were ${\alpha}$-endosulfan, ${\beta}$-endosulfan, and endosulfan sulfate, the residue were 2.0-12.0, 1.2-53.1, and $2.2-329.8{\mu}g/kg$, respectively. But these pesticides in all green perilla leaf and green pepper samples were not detected. CONCLUSION: These results showed that ROCPs residues in agricultural soils were not as high as crop safety threatening.

• Applied Chemistry for Engineering
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• v.27 no.4
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• pp.343-352
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• 2016

It has been estimated that the Earth has nearly 1.688 trillion barrels of crude oil, which will last 53.3 years at current extraction rates. The organization of petroleum exporting countries (OPEC) group forecasted that the oil prices will not jump to triple-digit territory within a decade, but it can quickly increase as the political issue for reducing oil production appears. With the potential of serious shortage of conventional hydrocarbon resources, the heavy oil, one of unconventional hydrocarbon resources including oil sand and natural bitumen has attracted worldwide interest. The heavy oil contains heavy hydrocarbon compounds, commonly called as resins and asphaltenes, with long carbon chains more than sixty carbon atoms. The high content of heavier fraction corresponds with the high molecular weight, viscosity, and boiling point. Physicochemical properties of residues from vacuum distillation of conventional oil, referred to as vacuum residues (VR) were similar to those of heavy oil. For the development of heavy oil reserves, reducing the heavy oil viscosity is the most important. In this article, commercially employed aquathermolysis processes and their application to VR upgrading are discussed. VR contains transition metals such as Ni and V, but these metals should be eliminated in advance for further refining. Recent studies on demetallization technologies for VR are also reviewed.

• Journal of Life Science
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• v.18 no.7
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• pp.974-979
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• 2008

The powdery mildew, a fungal plant disease found in varieties of plant cultures, is occurred by attack with Fusarium sp., Sphaerotheca sp., Leveilluna sp., and Eryshipe sp.. In this study we investigated the control of Fusarium graminearum, a barley powdery mildew fungus, by natural plant extracts. Among the 900 plant extracts tested, Zanthoxylum schinifolium, Ligusticum acutilobum, Bidens frondosa L., Dictamnus dasycarpus, Evodia officinalis, Disporum sessile, Scopolia japonica Max., Styrax japonica S. et Z., Dictamnus dasycarpus Turcz., Sinomenium acutum Rehder et Wils., Eugenia aromaticum, Rubus parvifolius L., Reynoutria elliptica, Coptis chinensis, Paeonia lactiflora Pall., Rheum undalatum, Paeonia suffruticosa, Oenothera odorata Jacq., Euphorbia pekinensis Rupr., and Nepeta cataria were selected based on spore germination inhibition assay. Further mycelial growth inhibition assay with economical and safety considerations led us to finally select Z. schinifolium (sancho) for control of F. graminearum. To produce antifungal sancho extract, methanol was suitable for extraction and subsequent fractionations of the extract showed that the water residue mainly had antifungal activity. The sancho extract and its fractions showed minor antibacterial activity against different pathogenic or food spoilage bacteria, but they did not show any harmful effects against young tomato plant by treatment of $1,000\;{\mu}g/ml$ in green chamber test. These results suggested that the extract of sancho has high potentials on control of a powdery mildew fungus, F. graminearum.

• 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.14 no.4
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• pp.361-370
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• 2010

Considering the efficiencies of the preparation process at each stage obtained in previous studies, the analytical determination method was established for multi-pesticide residues in soils. It consist of the acetone-extraction, the dichloromethane-partition, the Florisil or silica-gel chromatography and the gas chromatography analysis equipped with the electron capture detector and the nitrogen-phosphorus detector. In the soil recovery test by Florisil clean-up system, the number of pesticides recovered in the range of 70~120% and showed less than 20% of RSD were 165 pesticides for paddy soil, 169 pesticides for upland soil and 159 pesticides in both soils through the tested 183 pesticides. And in the soil recovery test by silica-gel system, the number of pesticides recovered in the range of 70~120% and showed less than 20% of RSD were 154 pesticides for paddy soil, 145 pesticides for upland soil, and 134 pesticides in both soils.

• Resources Recycling
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• v.19 no.4
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• pp.41-50
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• 2010

A fundamental study was carried out to develop a process for recycling tungsten and cobalt from WC-Co hardmetal sludge generated in the manufacturing process of hardmetal tools. The complete extraction of cobalt and simultaneous formation of tungstic was achieved by treating the sludge using aqua regia. The effect of aqua regia concentration, reaction temperature and time, pulp density on cobalt leaching and tungstic acid formation was investigated. The complete leaching of cobalt was attained at the optimum conditions: 100 vol.% aqua regia concentration, $100^{\circ}C$ temperature, 60 min. reaction time and 400 g/L pulp density. A complete conversion of tungsten carbide of the sludge to tungstic acid was however, obtained at the pulp densities lower than 150 g/L under the above condition. The progress of reaction during the aqua regia treatment of the sludge was monitored through the XRD phase identification of the residue. The metallic impurities in the tungstic acid so produced could be further removed as insoluble residues by dissolving the tungsten values in ammonia solution. The ammonium paratungstate($(NH_4)_{10}{\cdot}H_2W_{12}O_{42}{\cdot}4H_2O$) of 99.85% purity was prepared from the ammonium polytungstate solution by the evaporation crystallization method.

• The Korean Journal of Pesticide Science
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• v.12 no.4
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• pp.315-322
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• 2008

In this study, a simple, effective, and sensitive method has been developed for the quantitative residue analysis of cyhalofop-butyl and its metabolite cyhalofop acid in water and soil when kept under laboratory conditions. The content of cyholofop-butyl and cyhalofop acid in water and soil was analyzed by first purifying the compounds through liquid-liquid extraction and partitioning followed by Silica gel (adsorption) chromatography. Upon the completion of the purification step the residual levels were monitored through high-performance liquid chromatography (HPLC) using a UV absorbance detector. The recoveries of cyhalofop-butyl from three replicates spiked at two different concentrations ranged from 82.5 to 100.0% and from 66.7 to 97.9% in water and soil, respectively. The limit of detection and minimum detection level of cyhalofop-butyl in water and soil was 0.02 ppm and 10 ng, respectively. The recoveries of cyhalofop acid ranged from 80.7 to 104.8% in water and from 76.9 to 98.1 % in soil. The limit of detection of cyhalofop acid was 0.005 ppm in water and 0.01 ppm in soil, while the minimum detection level was 2 ng both in water and soil. The half-live of cyhalofop-butyl was 4.14 and 6.6 days in water and soil, respectively. The method was successfully applied to evaluate cyhalofop-butyl residues in water and soil applied aj. 30% emulsion, oil in water (EW) product.

• Journal of Food Hygiene and Safety
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• v.31 no.6
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• pp.432-438
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• 2016

Ethoxyquin (EQ, 1,2-dihydro-6-ethoxy-2,2,4-trimethyl-quinoline) is quinoline-based antioxidant used in the animal feed and food industry to protect the raw materials and final products against oxidation. In recent years the use of synthetic antioxidants in fishmeal ingredients carry-over to farmed fish fillets has received increasing attention in food safety. This study was conducted to develop an analytical method to determine EQ in aquatic products. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with 1 N HCl (in case of flatfish extracted with 1 N HCl containing 10% acetonitrile). Then, solid phase extraction (SPE) was used for the cleanup. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.99, analyzed at 0.005-0.2 mg/kg concentration. The developed method was validated according to the Codex Alimentarius Commission (CAC) guideline. The limits of quantitation for EQ were 0.01 mg/kg. Average recoveries ranged from 81.3% to 107%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was below 10%. The analytical method was characterized with high accuracy and acceptable sensitivity to meet CODEX guideline requirements and would be applicable to analyze the EQ residue in aquatic products.