• Journal of Korean Society on Water Environment
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• v.21 no.3
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• pp.219-229
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• 2005

The analytical methods for dioxins in water sample from wastewater to tap water were reviewed. For extraction method, liquid-liquid extraction (LLE) has been widely used, however, this process needs too much time and man power. New approach including solid phase extraction (SPE) is now applicable to large volume of water sample with high extraction efficiency. Column clean up in classical analytical methods were very complex and time consuming procedures during decade. Modifications were tried to decrease solvent and reagents volume. Moreover, use of column connection method has been demonstrated in the environmental matrices. Instrumental configurations also have been improved, in which GC/MS/MS with large volume injection approach can analyze picogram levels. Absolute sensitivities of HRMS increased compared to old versions of double focusing sector type mass spectrometers. Based on these analytical evolutions during last 10 years, we tried to optimize the analytical method for dioxins in water sample from sample extraction to instrumental analysis.

• Mass Spectrometry Letters
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• v.12 no.3
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• pp.112-117
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• 2021

α-Amanitin and β-amanitin are highly toxic bicyclic octapeptides responsible for the poisoning of poisonous mushrooms such as Amanita, Galerina, and Lepiota by inhibiting RNA polymerase II, DNA transcription, and protein synthesis. A sensitive, simple, and selective liquid chromatography-high resolution mass spectrometric method using parallel reaction monitoring mode was developed and validated for the simultaneous determination of α- and β-amanitin in mouse plasma to evaluate the toxicokinetics of α- and β-amanitin in mice. Protein precipitation of 5 μL mouse plasma sample with methanol as sample clean-up procedure and use of negative electrospray ionization resulted in better sensitivity and less matrix effect. The calibration curves for α- and β-amanitin in mouse plasma were linear over the range of 0.5-500 ng/mL. The intra- and inter-day coefficient of variations and accuracies for α- and β-amanitin at four quality control concentrations were 3.1-14.6% and 92.5-115.0%, respectively. The present method was successfully applied to the toxicokinetic study of α- and β-amanitin after an oral administration of α- and β-amanitin at 1.5 mg/kg dose to male ICR mice.

• Mass Spectrometry Letters
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• v.13 no.1
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• pp.20-25
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• 2022

Fargesin, a tetrahydrofurofuranoid lignan isolated from Flos Magnoliae, shows anti-inflammatory, anti-oxidative, anti-allergic, and anti-hypertensive activities. To evaluate the pharmacokinetics of fargesin in mice, a sensitive, simple, and selective liquid chromatography-high resolution mass spectrometric method using electrospray ionization and parallel reaction monitoring mode was developed and validated for the quantification of fargesin in mouse plasma. Protein precipitation of 6 µL mouse plasma with methanol was used as sample clean-up procedure. The standard curve was linear over the range of 0.2-500 ng/mL in mouse plasma with the lower limit of quantification level at 0.2 ng/mL. The intra- and inter-day coefficient variations and accuracies for fargesin at four quality control concentrations including were 3.6-11.3% and 90.0-106.6%, respectively. Intravenously injected fargesin disappeared rapidly from the plasma with high clearance values (53.2-55.5 mL/min/kg) at 1, 2, and 4 mg/kg doses. Absolute bioavailability of fargesin was 4.1-9.6% after oral administration of fargesin at doses of 1, 2, and 4 mg/kg to mice.

• Natural Product Sciences
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• v.28 no.1
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• pp.1-5
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• 2022

Two 2H-1-benzopyran derivatives, methyl 8-hydroxy-2,2-dimethyl-2H-1-benzopyran-5-carboxylate (1) and methyl 8-hydroxy-2,2-dimethyl-2H-1-benzopyran-6-carboxylate (2), including a new compound (1) were isolated from the twigs of Chaenomeles sinensis. Their chemical structures were characterized based on analysis of NMR data including ¹H and ¹³C, COSY, HSQC, and HMBC and HRMS data. The isolated compounds (1 and 2) were assessed for their anti-neuroinflammatory activity by measuring inhibition levels of nitric oxide (NO) production in lipopolysaccharide (LPS)-activated BV-2 cells and for their neurotrophic activity by the secretion of nerve growth factor (NGF) in C6 cells. Compounds 1 and 2 exhibited powerful anti-neuroinflammatory effects with IC₅₀ values of 17.14 and 19.30 μM, respectively, without cell toxicity, and also showed moderate effects on the stimulation of NGF secretion levels with 113.15 ± 3.54 and 130.20 ± 8.03%, respectively. The biosynthetic pathway of 1 and 2 was proposed that they would be derived from a protocatechuic acid and an isoprenyl unit.

• Journal of Environmental Health Sciences
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• v.41 no.1
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• pp.49-60
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• 2015

Objectives: Pine needles were used as a passive air sampler (PAS) of atmospheric persistent organic pollutants (POPs). This study was performed to investigate concentrations of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) deposited on pine needles near a waste incinerator and PCDD/Fs source contributions using principal component analysis (PCA). Methods: Two-year-old pine needles were sampled at 11 points with respect to distance and wind direction from the incinerator. PCDD/Fs deposited on pine needles were analyzed with HRGC/HRMS. The source contribution of PCA was calculated with SPSS. Results: The average concentration of PCDD/Fs deposited on pine needle was 0.79 (0.27-1.76) pg TEQ/g dry, PCDDs with 0.24 (0.01-0.95) pg TEQ/g dry and PCDFs with 0.56 (0.27-0.82) pg TEQ/g dry, respectively. The average concentration fraction of PCDDs was 29.7%, that of PCDFs was 70.3%, and PCDFs were more prevalent than PCDDs. The contributions of PCDD/Fs sources were estimated as incineration at 58.3% and automobiles at 28.4%. However, a relation and regulation between PCDD/Fs concentrations deposited on pine needles and distance from incinerator or wind direction was not shown. Conclusion: It was concluded that atmospheric PCDD/Fs concentrations near an industrial complex with a waste incinerator were affected by multiple sources. However, PCDD/Fs concentrations were lower than in other inland cities with the exception of background area.

• Bulletin of the Korean Chemical Society
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• v.26 no.4
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• pp.529-536
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• 2005

Measurement of toxicologically relevant polychlorinated biphenyl (PCB) congeners such as non-ortho(IUPAC#) 77, 81, 126, 169 and mono-ortho 105, 114, 118, 123, 156, 157, 189 and di-ortho 170, 180 and polybrominated diphenyl ethers (PBDEs) such as 47, 66, 85, 99, 100, 138, 153, 154 in environmental samples become almost mandatory in several countries now. However, most of the available methods involve expensive instrumentations such as HRGC-HRMS or ECNI-LRMS, apart from expensive extraction and clean-up (with large volume of solvents) steps. A method has been devised combining the analytical separation power of PYE [2-(1-pyrenyl)ethyldimethysilylated silica] column HPLC and high-resolution gas chromatographic techniques including micro-electron capture detection (ECD) and two dimensional gas chromatograpy-ECD techniques to determine these eco-toxic substances at parts-per-trillion (ppt) levels. This combination resolves co-elution of congeners that occur in disproportionate ratios (e.g. CB-110 and -77) and allows accurate congener-specific determination of target compounds. This method is cost effective as it requires only hexane, that in small quantities (10 mL) and GC-ECD. The elution and analysis time are optimized to less man hours. This method is effectively utilized in the analysis of co-planar PCBs and PBDEs from archived solvent extracts of samples previously analyzed for pesticides and PCBs. Structure based separation of contaminant classes improves GCECD determination at ppt levels.

• Smart Structures and Systems
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• v.22 no.2
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• pp.185-192
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• 2018

Participants in the Asia Pacific Conference of the Prognostics and Health Management Society 2017 (PHMAP 2017) Data Challenge were given measured vibration signals from motor-driven gearboxes used in pulverizers. Using this information, participants were requested to predict failure dates and the faulty components. The measured signals were affected by significant noise and disturbance, as the pulverizers in the provided data worked under actual operating conditions. This paper thus presents a fault prediction method for a motor-driven gearbox in a pulverizer system that can perform under external noise and disturbance conditions. First, two fault features, an RMS value in the higher frequency zones (HRMS) and an amplitude of a period for high-speed shaft in the quefrency domain ($QA_{HSS}$), were extracted based on frequency analysis using the higher and lower sampling rate data. The two features were then applied to each pulverizer based on results of frequency responses to impact loadings. Then, a regression analysis was used to predict the failure date using the two extracted features. A weighted regression analysis was used to compensate for the imbalance of the features in the given period. In addition, the faulty components in the motor-driven gearboxes were predicted based on the modulated frequency components. The score predicted by the proposed approach was ranked first in the PHMAP 2017 Data Challenge.

• Korean Journal of Environmental Agriculture
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• v.31 no.3
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• pp.255-263
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• 2012

BACKGROUND: The analysis for the concentration and enantiomeric ratio of OCPs have been performed to confirm the distribution and to emonstrate the pollution characteristics of chiral OCPs in ambient air. METHODS AND RESULTS: In ambient air at coastal and inland sites, concentrations and enantiomer fractions (EFs) of heptachlor (HEPT), eptachlor epoxide (HEPX), trans-chlordane (TC), cis-chlordane (CC), xychlordane (OXY), 2,4'-DDT, 2,4'-DDD with HRGC/HRMS were investigated to understand source and distribution of chiral organochlorine pesticides (OCPs) in ambient air. The mean concentrations of OCPs in ambient air were at the range of 0.027(heptachlor)~1.279 (4,4'-DDT) pg/m3 and 0.0005 (heptachlor)~0.1043 ng/g d.w. (TC), respectively. The mean EFs of OCPs in ambient air were at the range of 0.73 (HEPX)~0.45 (CC). Both preferential depletions of (+) and (-) enantiomer were observed for CC, indicated by EFs either <0.5 or >0.5, while preferential depletions of (-) enantiomer which mean EFs <0.5 were observed for chiral OCPs except TC and MC-5. CONCLUSION: OCPs in ambient air have been distributed from soil, but some of them such as chlordane, DDT etc. might have been introduced by long-range atmospheric transport, considering EFs by chiral analysis and trajectory analysis.

• Analytical Science and Technology
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• v.15 no.2
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• pp.142-148
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• 2002

They were analyzed that the levels of PCDDs/PCDFs in mackerel, walleye pollack, croaken and cuttlefish, which were mainly consumed in Korea, by high resolution gas chromatography/high resolution mass spectrometr (HRGC/HRMS). The samples measured in this study had been bought 3 sets of each fish from different 5 cities, Seoul, Chunchon, Daejon, Kwangju and Pusan. The TEQ level of PCDDs in mackerel (0.032 pgTEQ/g) was the highest. The TEQ level of PCDFs in walleye pollack (0.010 pgTEQ/g) was the lowest. The level of PCDDs was higher than PCDFs in fish.

• Journal of Environmental Health Sciences
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• v.40 no.3
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• pp.215-224
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• 2014

Objective: This study was carried out in order to determine the depositional characteristics of pine needles, pine bark, and soil used as a passive air sampler (PAS) for atmospheric polybrominated diphenyl ethers (PBDEs). Methods: All three media were sampled from the same site. The PBDE concentrations were analyzed by HRGC/HRMS, and the lipid contents were measured using the gravimetric method by n-hexane extraction. Results: The total PBDE concentration was the highest in soil (22,274.57 pg/g dry), followed by pine bark (20,266.39 pg/g dry), and then pine needles (7,380.22 pg/g dry). Pine needles contained the highest lipid contents (21.31 mg/g dry), whereas soil (10.01 mg/g dry), and pine bark (4.85 mg/g dry) contained less. There were poor correlations between lipid content and total PBDE concentrations in the media ($R^2$=0.8216, p=0.2814). Congeners BDE 47, 99, 183, 196, 197, 206, 207 and 209 showed peak concentrations. Among these, BDE 206, 207, and 209 are highly brominated PBDEs that exist as particulates in ambient air. They accounted for 81.2% [69.2 (pine needles) - 89.0% (tree bark)] of the concentration and therefore are noted as the main congener of the total PBDEs. Conclusions: It can therefore be concluded that for reducing error by improper sampling, the same species of media should be recommended for use as a PAS for atmospheric PBDEs due to the differences in depositional characteristics.