• 분석과학
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• 제14권1호
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• pp.21-27
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• 2001

본 실험에서는 유도결합 플라스마 원자방출 분광법 (ICP-AES)에서 perfluoroalkoxy (PFA) nebulizer와 microconcentric nebulizer (MCN)을 이용하여 본 실험실에서 제작된 double membrane desolvator (DMD)의 분석능력을 연구하였다. MCN과 비교하여 PFA nubulizer는 수용액 시료의 경우에는 DMD-ICP-AES에서 비슷한 분석감도를 보였으나, isopropyl alcohol 시료에서는 좀 더 나은 분석감도를 보였다. PFA nebulizer는 여러 가지 산들에 견디기 때문에 HCI, $H_2SO_4$ 뿐만 아니라 HF 용액도 도입하여 분석할 수 있었는데, 모두 2% 미만의 상대표준편차로 분석되었다. 기억효과를 측정한 결과, 신호가 1% 미만으로 감소되는 rinse-out time은 PFA에서는 35초인 반면 MCN은 45초로 얻어졌다.

• Mass Spectrometry Letters
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• 제6권4호
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• pp.116-119
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• 2015

Globotriaosylsphingosine (lyso-Gb3) is considered as one of the biological marker for Fabry disease. To date, a reliable biomarker that reflects disease severity and progression has not been discovered to guide the management of Fabry disease. A new method included a simple protein precipitation with acetonitrile in 100 μL of plasma following analyte separation on an Phenomenex Kintex- C18 column using a gradient elution (0.1% formic acid in 5-90% acetonitrile). Total run time was within 12 min including sample preparation and MS/MS analysis. The limit of detection and limit of quantitation were 1 ng/mL and 2 ng/mL, respectively. The calibration curve was linear over the concentration range of 2.0-200.0 ng/mL (r² = 0.9999). Inter-day accuracy and precision at 7 level were 93.4-100.7% with RSD of 0.55-5.97%. Absolute recovery was 97.6-98.6%. The method was applied to human and mice plasma, proved the suitability for quantification of lyso-Gb3 for screening, diagnosis and therapeutic monitoring of Fabry disease patients.

• 한국연초학회지
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• 제36권1호
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• pp.12-19
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• 2014

A matrix solid-phase dispersion (MSPD) method was developed for extracting and cleaning-up the selected agrochemicals in tobacco using gas chromatography-mass spectrometry with selected ion monitoring (GC/MS-SIM). Different parameters of the method were investigated and optimized, such as the type of solid-phase (alumina, $C_{18}$ and Florisil) and eluent (acetone, acetonitrile, ethylacetate and n-hexane). The best results were obtained using 0.5 g of tobacco sample, 1.0 g of $C_{18}$ as dispersant sorbent, 1.0 g of Florisil as clean-up sorbent and acetonitile saturated with n-hexane as eluting solvent. The method was validated using tobacco samples fortified with agrochemicals at their different concentration levels. This method gave good linearity for the selected agrochemicals of ranging from $0.01{\mu}g/mL$ to $0.1{\mu}g/mL$. Recoveries of the selected agrochemicals in tobacco were more than 80 % and reproducibilities were found to be better than 10 % RSD. Those results suggested that the analytical procedure including MSPD method in combining with GC/MS could be applicable to the rapid determination often the selected agrochemicals in tobacco.

• 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.

• BMB Reports
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• 제45권4호
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• pp.233-238
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• 2012

We present a top down separation platform for yeast ribosomal proteins using affinity chromatography and capillary electrophoresis which is designed to allow deposition of proteins onto a substrate. FLAG tagged ribosomes were affinity purified, and rRNA acid precipitation was performed on the ribosomes followed by capillary electrophoresis to separate the ribosomal proteins. Over 26 peaks were detected with excellent reproducibility (<0.5% RSD migration time). This is the first reported separation of eukaryotic ribosomal proteins using capillary electrophoresis. The two stages in this workflow, affinity chromatography and capillary electrophoresis, share the advantages that they are fast, flexible and have small sample requirements in comparison to more commonly used techniques. This method is a remarkably quick route from cell to separation that has the potential to be coupled to high throughput readout platforms for studies of the ribosomal proteome.

• 생약학회지
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• 제40권3호
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• pp.224-228
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• 2009

For the quality control of traditional herbal medicine, Galgeun tang, simultaneous determination of glycyrrhizin, paeoniflorin, puerarin, 6-gingerol was established by using a high performance liquid chromatographic (HPLC) method with diode array detector. To separate five four constituents, DIONEX $C_{18}$ column ($5{\mu}m$, $120{\AA}$, $4.6\;mm{\times}150\;mm$) was used with gradient elution system of water and methanol. Validation of the chromatography method was evaluated by linearity, recovery, and precision test. Calibration curve of standard components showed excellent linearity ($R^2$>0.9906). Limits of detection (LOD) and limits of quantification (LOQ) varied from 0.15 to $0.52{\mu}g$/ml and 0.27 to $0.80{\mu}mg$/ml, respectively. The relative standard deviations (RSDs) of data of the intra-day and inter-day experiments were less than 2.88% and 1.21%, respectively. The results of recovery test were ranged from 96.71 to 106.29% with RSD values 0.01-0.80%.

• 대한화학회지
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• 제31권5호
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• pp.425-433
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• 1987

모세관 컬럼을 사용한 기체크로마토그래피로 19종 유기염소제 농약의 분리를 검토하였고, 쌀에 첨가한 농약들의 회수율을 구하여 봄으로써 실제분석에 대한 본 방법의 응용 가능성을 조사하였다. SE-30과 OV-17모세관 컬럼의 분리를 비교하여 본 결과 OV-17 컬럼(25m ${\times}$ 0.20mm, 0.27${\mu}$m 두께)으로 분리가 잘되고 있으며, splitless방식으로 주입한 농약들의 머무른 시간과 봉우리 면적에 대한 상대표준 편차가 최대로 0.16%와 8.2%이었다. 쌀에 첨가된 농약의 회수율은 대부분 85%이상이었고 분석 결과에 대한 상대표준편차가 가장 큰 것이 11.4%로서 흔적량의 잔류농약분석에서 비교적 정밀도가 좋음을 확인하였다.

• 대한전기학회:학술대회논문집
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• 대한전기학회 1995년도 추계학술대회 논문집 학회본부
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• pp.348-351
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• 1995

A modified silicon direct bonding method has been developed alloying an intimate contact between grooved and smooth mirror-polished oxide-free silicon wafers. A regular set of grooves was formed during preparation of heavily doped $p^+$-type grid network by oxide-masking und boron diffusion. Void-free bonded interfaces with filing of the grooves were observed by x-ray diffraction topography, infrared, optical. and scanning electron microscope techniques. The presence of regularly formed grooves in bending plane results in the substantial decrease of dislocation over large areas near the interface. Moreover two strongly misoriented waters could be successfully bonded by new technique. Diodes with bonded a pn-junction yielded a value of the ideality factor n about 1.5 and the uniform distribution of series resistance over the whole area of horded pn-structure. The suitability of the modified technique was confirmed by I - V characteristics of power diodes and reversly switched-on dynistor(RSD) with a working area about $12cm^2$. Both devices demonstrated breakdown voltages close to the calculation values.

• 한국대기환경학회지
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• 제22권2호
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• pp.201-208
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• 2006

Several carbonyl compounds are important because of their irritant and toxic properties, mutagenicity and carcinogenicity. Therefore, they are regulated in korean odor emission standard. In this study, atmospheric pressure ionization-mass spectrometry(API-MS) is used for the analysis of carbonyl compounds after derivatization with 2, 4-dinitrophenylhydrazine (DNPH) and liquid chromatographic separation. In the negative ion mode, the $[M-H]^-$ pseudomolecular ions are most abundant for the carbonyls. Analytical parameters such as linearity, repeatability and minimum detection limit were evaluated. The linearities ($r^2$) for carbonyls were $0.9977{\sim}0.9999$ when analyte concentration ranges from $25\;to\;250{\mu}g/L$(n=6). The relative standard deviations (%RSD) for carbonyls were $0.55{\sim}3.51%$ for concentration of $100{\mu}g/L$(n=5). The minimum detection limit (MDL) was $1.88{\mu}g/L$(0.27 ppb) for i-valeraldehyde. It was shown that LC-MS method has a great potential for carbonyl compounds analysis.

• 한국연초학회지
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• 제28권1호
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• pp.51-57
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• 2006

This study was carried out to improve and evaluate the analytical method for determination of potassium in tobacco leaf by various pre-treatment techniques. The time requirment of various pre-treatments was about 10 hour for dry ashing and 6 hour for microwave digestion and 3 hour for sonication. The results of recover in both pre-treatment techniques, microwave digestion and sonication, is greater than 85 % stably with reproducibility(RSD %) on replicates of less than 3 %. However the mean values for microwave digestion were lower than certified standard value of NlST SRM. Compared to the other pre-treatment techniques, analytical results for sonication technique strictly improved the accuracy and precision. In conclusion, the use of the simple sonication technique seems to be efficient for the determination of potassium in tobacco leaf in consideration for both the accuracy and reproducibility.