• 한국환경과학회지
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• 제18권12호
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• pp.1369-1381
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• 2009

The simultaneous determination of residual pesticides was developed using a gas chromatography. In this study, a simple and reliable methodology was improved to detect 175 kinds of residual pesticides by a liquid-liquid extraction procedure, followed by chromatographic analysis by gas chromatography. The 175 kinds of residual pesticides was classified into 4 groups according to the chemical structure, column type, resolution and sensitivity. The soybean sample selected for recovery experiment was not detected any pesticides. The recovery rates were ranged from 70.6% to 119.7% in most pesticides. The relative standard deviation (RSD 0.3~5.6%) was lower than 5.6% in all cases. The limits of detection (LOD) was lower than the maximum residue levels established by Korean legislations. The method has been successfully applied to the analysis of approximately 130 real samples.

• Journal of Radiation Protection and Research
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• 제22권3호
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• pp.161-170
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• 1997

현재 한국원자력연구소에서 개인방사선피폭관리용으로 사용되고 있는 C-300-A $CaSO_4$:Dy 열형광선량재의 최소검출한계(LLD)를 계산 및 실험에 의하여 구하였으며, 이때 오차의 확율이 자연방사선의 측정변화에 기인되는 선량준위로 정의되는 임계준위도 함께 구하였다. 개인방사선피폭서비스를 수행하는 기관에서는 이를 이용하여 개인선량계 패용 기간동안의 자연방사선 판독결과와 기지의 선량을 조사시킨 선량제의 판독결과로부터 쉽게 LLD를 구할수 있다. 또한 3개월간에 걸쳐 온도 및 습도의 변화에 따른 개인선량제의 잠상퇴행률을 실험적으로 구하였다. 마지막으로 40회 연속사용시 개인선량계의 반복사용에 의한 감도변화를 측정하였다. 본 실험결과 얻어진 잠상퇴행률과 연속사용시의 감도변화를 실제 개인방사선피폭 평가시 적용방법에 대하여 간략하게 논의하였다.

• Journal of Periodontal and Implant Science
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• 제26권1호
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• pp.161-175
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• 1996

There were many reports that elevations in the levels of active and latent collagenase in gingival crevicular fluid(GCF) have been correlated positively with periodontal disease activity. To provide a simple diagnostic approach for testing GCF collagenolytic activity, the detection limit of enzyme activity was compared using radiofibril assay(Sodek et.al.1981) and spectrophotometric collagenolytic assay(Nethery et al. 1986). The detection limits of both assay for standard bacterial enzyme were similar and the radiofibril assay showed a little (1/2) lower detection limit for tad pole collagenase. To evaluate the relationship between periodontal tissue destruction and the collagenolytic activity, GCF was collected, and latent and active enzyme activities were measured by a spectrophotometric collagenolytic assay. Twelve subjects showing progressive lesions were selected according to the presence of immediate tissue destruction, frequent abscess formation, and increasing need for tooth extraction, and the absence of underlying systemic disease and previous antibiotic medication history within 6 months. Comparisons were made between sites with either: 1) inflammation with a previous history of progressive loss of periodontal tissue and bone support(2l progressive sites): 2) previous history of bone loss and periodontal destruction but now clinically stable(12 comparably stable sites); or 3) no loss of periodontal tissue and bone support(11 control sites including 5 gingivitis sites and 6 healthy sites). Active collagenase activity was the highest in the progressive sites and decreased in the order of the gingivitis sites, the stable sites, and the healthy sites. The total enzyme activity was $2{\sim}3$ fold higher in the progressive sites and the gingivitis sites, compared to the stable and the healthy sites. The ratio of active to total collagenolytic activity was twice in the progressive sites. Analysis of active collagenase level(5mU) and the ratio of active to total collagenolytic activity(0.8) as a diagnositic test indicates that these measurements have the sensitivity of 0.81 and 0.86, the specificity of 0.70 and 0.65, and the overall agreement of 0.75 and 0.73, respectively. Thus, this method has significant merits as a diagnostic tool to determine wherher the site is in a state of remission or progression.

• Toxicological Research
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• 제26권2호
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• pp.149-155
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• 2010

The pesticide trichlorfon is readily degraded under experimental conditions to dichlorvos. A method has therefore been developed by which residues of trichlorfon in milk are determined as dichlorvos, using gas chromatography with ${\mu}$-electron capture detection. The identification of dichlorvos was confirmed by mass spectrometry. Milk was extracted with acetonitrile followed by centrifugation, freezing lipid filtration, and partitioning into dichloromethane. The residue after partitioning of dichloromethane was dissolved in ethyl acetate for gas chromatography. Recovery concentration was determined at 0.5, 1.0, and 2.0 of times the maximum permitted residue limits (MRLs) for trichlorfon in milk. The average recoveries (n = 6) ranged from 92.4 to 103.6%. The repeatability of the measurements was expressed as relative standard deviations (RSDs) ranging from 3.6%, to 6.7%. Limit of detection (LOD) and limit of quantification (LOQ) were 3.7 and $11.1{\mu}g/l$, respectively. The accuracy and precision (expressed as RSD) were estimated at concentrations from 25 to $250{\mu}g/l$. The intra- and inter-day accuracy (n = 6) ranged from 89.2% to 91% and 91.3% to 96.3%, respectively. The intra- and inter-day precisions were lower than 8%. The developed method was applied to determine trichlorfon in real samples collected from the seven major cities in the Republic of Korea. No residual trichlorfon was detected in any samples.

• KSBB Journal
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• 제25권1호
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• pp.85-90
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• 2010

An ion selective microelectrode (ISME) was fabricated to measure concentrations of ammonium (${NH_4}^+$-N) and nitrate (${NO_3}^-$-N) according to the depth of nitrifying biofilm. The limits of detectability and validity of results were investigated to evaluate the ISME. The electromotive force (EMF) was directly proportional to the ion concentration, and average detection limits of ${NH_4}^+$ and ${NO_3}^-$ ISME were $10^{-5.14}$ and $10^{-5.18}$ M, respectively. The concentrations of ${NH_4}^+ $-N and ${NO_3}^-$-N in various depths on the nitrifying biofilm were measured by the ISME. When a modified Ludzack-Ettinger (MLE) process was operated at an HRT of 6 h, concentration gradients of ${NH_4}^+$-N in the bulk solution and biofilm at depths of $100\;{\mu}m$ decreased by $70\;{\mu}M$, while ${NO_3}^-$-N increased by $101\;{\mu}M$ and remained constant thereafter. At an HRT of 4 h, concentration gradients of ${NH_4}^+$-N at depths of $500\;{\mu}m$ decreased by $160\;{\mu}M$ and ${NO_3}^-$-N increased by $162;{\mu}M$ and remained constant thereafter. As HRT decreased, the concentration gradients of ${NH_4}^+$-N and ${NO_3}^-$-N between bulk solution and biofilm was higher due to the increase of nitrogen load. Also, the concentration gradients of the ${NH_4}^+$-N and ${NO_3}^-$-N of biofilm in the second aerobic tank were lower than those of the first aerobic tank, suggesting differences of nitrogen load and concentrations of DO between the first and second aerobic tank.

• 약학회지
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• 제40권2호
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• pp.135-140
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• 1996

Ion-selective poly(vinyl chloride)(PVC) membrane electrodes for the determination of the calcium antagonist verapamil and its pharmaceutical preparations were described. Verapam il-superchrome garnet Y(SGY), lumogallion(LG), acid red 97(AR97), Dragendorff(DD) and Meyer reagent ion pairs were inverstigated as an electroactive compound for membrane electrode. Stable potentiometric response was obtained with azo dye at pH 6.5-4.0 and with DD, and Meyer reagent at pH 6.5-3.0. The best plasticizer was 49w/w% 2-nitrophenyl octyl ether for azo dye, and 65.3w/w% tri(n-butyl) citrate for DD and Meyer reagent. Potentiometric response slopes of optimized membrane electrodes based on SGY, LG, AR97, DD, and Meyer complex for verapamil were 52.49, 54.88, 50.81, 54.13 and 49.31 mV/dec., respectively. Lower limits of linear range were $1.0{\times}10^6M$ for SGY, LG, and AR97, while those for DD and Meyer reagent were $4{\times}10^{-6}M$. Detection limits for all these electrodes were $1{\times}10^{-5}M,\;4{\times}10^{-6}M,\;1.8{\times}10^{-6}M,\;8{\times}10^{-7}M,\;and\;1{\times}10^{-6}M$ with relative standard deviation of 2.56, 3.6, 3.96, 2.56, 3.20%, respectively.

• Archives of Pharmacal Research
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• 제25권5호
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• pp.647-651
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• 2002

An LC/MS/MS method for the simultaneous determination of a neuroprotective agent for ischemia-reperfusion damage, KR-31378 and its N-acetyl metabolite KR-31612 in human plasma was developed. KR-31378, KR-31612 and the internal standard. KR-31543 were extracted from human plasma by liquid-liquid extraction. A reverse-phase HPLC separation was performed on Luna phenylhexyl column with the mixture of acetonitrile-5 mM ammonium formate (55:45, v/v) as mobile phase. The detection of analytes was performed using an electrospray ionization tandem mass spectrometry in the multiple reaction monitoring mode. The lower limits of quantification for KR-31378 and KR-31612 were 2.0 ng/ml. The method showed a satisfactory sensitivity, precision, accuracy, recovery and selectivity.

• Environmental Analysis Health and Toxicology
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• 제17권2호
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• pp.95-107
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• 2002

This study was designed to investigate the characteristics of atmospheric concentrations of toxic volatile organic compounds (VOCs) in Korea. Target compounds included 1,3-butadiene, aromatics such as BTEX, and a number of carbonyl compounds. In this paper, as the first part of the study, the performance of sampling and analytical methods was evaluated for the measurement of selected VOCs and carbonyl compounds in the ambient air. VOCs were determined by the adsorbent tube sampling and automatic thermal desorption coupled with GC/MSD analysis, while carbonyls by the DNPH-silica cartridge sampling with HPLC analysis. The methodology was investigated with a wide range of performance criteria such as repeatability, linearity. lower detection limits, collection efficiency, thermal conditioning, breakthrough volume and calibration methods using internal standards. In addition, the sampling and analytical methods established in this study were applied to real field samples duplicately collected in various ambient environments. Precisions for the duplicate samples appeared to be comparable with the performance criteria recommended by USEPA TO-17. The overall precision of the sampling and analytical methods was estimated to be within 20 ∼ 30% for major aromatic VOCs such as BTEX, whereas the precision for major carbonyl compounds such as formaldehyde and acetaldehyde was within 10 ∼ 20% for field samples. This study demonstrated that the adsorbent sampling and thermal desorption method can be reliably applied for the measurement of BTEX in ppb levels frequently occurred in common indoor and ambient environments.

• 한국대기환경학회지
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• 제22권3호
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• pp.297-307
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• 2006

During January $2002{\sim}April\;2004$, hydrogen peroxide ($H_{2}O_{2}$) measurements were performed at the campus of Korea University, which is located in the northeastern part of Seoul. Gas phase hydroperoxide was collected in aqueous solution and separated by HPLC. Concentrations were determined by fluorescence using postcolumn enzyme derivatization. This measurement system was improved to be run automatically from sample collection at every 10 minutes through chemical analysis for data collection. Detection limits of $H_{2}O_{2}$ is $10{\sim}17\;pptv$, and the overall uncertainty of the measurements is better than 8%. Two-year measurements of $H_{2}O_{2}$ show typical seasonal variations. Concentrations of $H_{2}O_{2}$ were higher during $June{\sim}October$ and lower during $January{\sim}February$. Maximum concentration of 1-hour averaged $H_{2}O_{2}$ was 6.5 ppbv, which was observed in August and September. In general $H_{2}O_{2}$ concentrations were well correlated with $O_{3}$ concentrations and largely affected by meteorological factors such as temperature and wind direction.

• 한국축산식품학회지
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• 제41권4호
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• pp.731-738
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• 2021

Herein, a novel analytical method using a high-performance liquid chromatography-fluorescence detector (HPLC/FLD) is developed for rapidly measuring an L-carnitine ester derivative in infant powdered milk. In this study, solid-phase extraction cartridges filled with derivatized methanol and distilled water were used to effectively separate L-carnitine. Protein precipitation pretreatment was carried out to remove the protein and recover the analyte extract with a high recovery (97.16%-106.56%), following which carnitine in the formula was derivatized to its ester form. Precolumn derivation with 1-aminoanthracene (1AA) was carried out in a phosphate buffer using 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) as the catalyst. Method validation was performed following the AOAC guidelines. The calibration curves were linear in the L-carnitine concentration range of 0.1-2.5 mg/L. The lower limit of quantitation and limit of detection of L-carnitine were 0.076 and 0.024 mg/L, respectively. The intra- and interday precision and recovery results were within the allowable limits. The results showed that our method helped reduce the sample preparation time. It also afforded higher resolution and better reproducibility than those obtained by traditional methods. Our method is suitable for detecting the quantity of L-carnitine in infant powdered milk containing a large amount of protein or starch.