• Bulletin of the Korean Chemical Society
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• 제28권1호
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• pp.59-62
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• 2007

A quantitative analysis method of halogen elements in volatile organohalogen compounds was established by the Wickbold combustion pretreatment in an enclosed system and ion chromatography. The sample pretreatment parameters of Wickbold combustion were experimentally optimized, and using the determined optimal pretreatment parameters, the reproducibility was estimated by ion chromatography. As a comparison for real samples, NIST certified reference materials (CRMs) were analyzed for the recovery efficiency and reproducibility.

• Bulletin of the Korean Chemical Society
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• 제33권12호
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• pp.3971-3976
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• 2012

A simple method was developed for the analysis of seven stilbene-type fluorescent whitening agents (FWAs) in paper materials by ion-pair reversed-phase high-performance liquid chromatography with fluorescence detection. These stilbene-type FWAs included two disulfonate, two tetrasulfonate, and three hexasulfonate compounds. After optimization of chromatographic conditions, the FWAs were satisfactorily separated using a reversed-phase column (RP-18) with the following isocratic mobile phase: methanol-water (60:40) containing 17.5 mM TBABr and 10 mM citrate buffer (pH = 7.0). The calibration plot was linear in the range from 5 to 500 ng/mL for two disulfo-FWAs and from 1 to 500 ng/mL for the other five FWAs. Precision levels of the calibration curve as indicated by RSD of response factors were 1.2 and 8.1%. Limits of quantitation (LOQ) ranged from 1.2 to 11 ng/mL.

• Journal of the Korean Wood Science and Technology
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• 제21권3호
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• pp.22-29
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• 1993

나뭇잎으로부터 발생되는 저분자량 유기산을 이온크로마토그래피를 이용하여 분석하였다. 이 방법은 자연상태의 나뭇잎 (needle litter)을 유기용매의 추출 없이 그대로 이용할 수 있어서 사용하기에 편리하다. 본 논문에서는 이온 크로마토그래피의 사용방법과 침엽수잎(Pacific Silver Fir)의 부후정도에 따른 유기산의 종류와 농도의 변이를 간략하게 소개한다. 초기의 침엽수잎 여과액으로부터는 $C_2$에서 $C_4$까지의 아세트산(acetic acid), 프로피온산(propionic acid), 옥살산(oxalic acid) 그리고 포름산(formic acid) 등이 주종을 이루지만 부후정도가 커짐에 따라 방향핵을 가진 방향핵 유기산(aromatic organic acid)이 발생한다.

• Mass Spectrometry Letters
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• 제5권1호
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• pp.24-29
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• 2014

An advanced and reliable high performance liquid chromatography (HPLC)/ultraviolet detector (UV)/ion-trap time-of-flight (IT-TOF) mass spectrometry was developed for the simultaneous quantification of 19 marker compounds in Bang-poong-tong-sung-san (BPTS), a traditional oriental prescription. Various parameters affecting HPLC separation and IT-TOF detection were investigated, and optimized conditions were identified. The separation was achieved on a Capcell PAK C18 column ($1.5mm{\times}250mm$, $5{\mu}m$ particle size) using a gradient elution of acetonitrile and water containing 0.1% formic acid at a flow rate of 0.1 mL/min. The column temperature was maintained at $40^{\circ}C$ and the injection volume was $2{\mu}L$. IT-TOF system was equipped with an electrospray ion source (ESI) operating in positive or negative ion mode. The optimized electrospray ionization parameters were as follows: ion spray voltage, +4.5 kV (positive ion mode), or -3.5 kV (negative ion mode); drying gas ($N_2$), 1.5 L/min; heat block temperature, $200^{\circ}C$. Automatic $MS^n$ (n = 1~3) analyses were carried out to obtain structural information of analytes. Elemental compositions and their mass errors were calculated based on their accurate masses obtained from a formula predictor software. The marker compounds in BPTS were identified by comparisons between $MS^n$ spectra from standards and those from extracts. Moreover, the libraries of $MS^2$ and $MS^3$ spectra and accurate masses of parent and fragment ions for marker compounds were constructed. The developed method was successfully applied to the BPTS extracts and identified 17 out of 19 marker compounds in the BPTS extracts.

• Journal of Microbiology and Biotechnology
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• 제3권3호
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• pp.161-167
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• 1993

Immobilized metal ion affinity chromatography (IMAC) was used to separate various types of recombinant hirudins from the culture broth. The wild type hirudin exhibited a retention in Cu(II)-chelated affinity chromatgoraphy since it contained a single exposed histidine at position 51. To obtain a stronger retention on an IDA-Cu(II) column, the hirudin variants were genetically engineered to contain one or two histidine (s) more than the wild type. While the affinity of the variants for IDA-Cu(II) ligand increased in comparison to that of the wild type, the antithrombin activities reduced to a certain degree. Cu(II), Ni(II) and Zn(II) ions were applied separately to the metal chelate column to investigate ligand specificity with respect to protein retention. As a result, the Cu(II) chelated chromatography gave the best resolution for all the hirudins tested and appeared to be the only IMAC that could be used generally for the purification of hirudins with a decreasing pH gradient.

• 분석과학
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• 제21권4호
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• pp.284-295
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• 2008

플라스틱 시료 중 각종 유해물질 유무 확인을 위한 여러 가지 시험항목을 저비용으로 빠르게 분석할 수 있는 방법으로 Combustion ion chromatography(연소IC)를 사용한 방법을 채택하였다. F, Cl 및 Br의 3개 항목에 대하여 연소IC로 시험법 유효화 검증을 실시한 결과, 검량선은 0.5~4.0 mg/kg 농도범위에서 $r^2$ = 0.999~1.000의 상관관계 계수를 갖는 좋은 직선성을 나타내었으며, 검출한계는 0.005~0.024 mg/kg, 정량한계는 0.014~0.073 mg/kg 이였다. 인증표준물질(CRM)을 사용한 연소IC의 회수율은 95.5~104.9%이었다. 본 결과를 토대로 국내외 시험기관간 비교 숙련도 시험을 실시하였으며, 그 결과 연소IC 방법이 전기전자제품 중에 halogen-free 및 기타 유해물질 규제 대응을 위한 효율적인 분석방법임을 확인하였다.

• Environmental Analysis Health and Toxicology
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• 제16권3호
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• pp.121-126
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• 2001

Analytical method of benzophenone (BP) in sediment and soil was developed by gas chromatography/mass selective detector/selected ion monitoring (GC/MSD/SIM). The ultrasonic extraction of US EPA (method 3550B) method and liquid-liquid extraction for sediment and soil samples were used for the analysis of BP from sediment and soil. BP was extracted with n-hexane. Organic layer was washed with 5% sodium chloride solution. 1∼2 l of the concentrated solution of organic layer was applied to GC/MSD. The retention time of BP peak was 11.10 min. Recovery (％) of BP by ultrasonication from sediment and soil samples was 96.0∼100.6％ and 40.0∼83.0％, respectively. Recovery of BP by liquid-liquid extraction was 51∼59％ in soil samples. The detection limit of BP in sediment and soil samples were determined to 0.1 ng/g.

• Archives of Pharmacal Research
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• 제19권5호
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• pp.396-399
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• 1996

High-performance liquid chromatographic method with UV detecction was developed for the determination of theophylline and its metabolites in human urine using ${beta}$-hydroxyethyl theophylline$({beta} -HET)$ as an internal standard. For extraction of urine sample, quality control sample and xanthine-free blank urine were mixed with decylamine (ion-paring reagent) and ${beta}$-HET. After saturation with ammonium sulfate, the mixture was then extracted with organic solvent at pH values of 4.0-4.5. All separations were performed with ion-pair chromatography using decylamine as an ion-pairing reagent and 3mM sodium acetate buffered mobile phase (pH 4.0) containing 1% (v/v) acetonitrile and 0.75 mM decylamine. The detection limits of theophylline, 1, 3-DMU, 1-MU, 3-MX and 1-MX in human urine were 0.17, 0.17, 0.39, 0.19 and 0.19 ${\mu}g$/ml, based on a signal-to-noise ratios of 3.0. The mean intraday coefficients of variation (C.V.s) of each compound on nine replicates were lower than 2.0%, while mean interday C.V.s on three days were lower than 1.6%. All separations were finished within 40miutes.

• Safety and Health at Work
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• 제12권2호
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• pp.209-216
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• 2021

Background: The article presents the results of studies performed in order to develop a new method of airborne potassium bromate(V) determination at workplaces. Methods: The method is based on a collection of the inhalable fraction of potassium bromate(V) using the IOM Sampler, then extraction of bromates with deionized water and chromatographic analysis of the obtained solution. The analysis was performed using ion chromatography with conductometric detection. The tests were performed on a Dionex IonPac®AS22 analytic column (250 × 4 mm, 6 ㎛) with AG22 precolumn (50 × 4 mm 11 ㎛). Results: The method provides for potassium bromate(V) determination within the concentration range of 0.043 ÷ 0.88 mg/m³ for an air sample of 0.72 m³ in volume, i.e., 0.1-2 times the exposure limit value as proposed in Poland. The method was validated in accordance with PN-EN 482. The obtained validation data are as follows: measuring range: 3.1-63.4 ㎍/mL, limit of detection (LOD) = 0.018 ㎍/mL and limit of quantification (LOQ) = 0.053 ㎍/mL. The developed method has been tested in the work environment, on laboratory employees having contact with potassium bromate(V). Conclusion: The analytical method allowed the determination of the inhalable fraction of airborne potassium bromate(V) at workplaces and can be used to assess occupational exposure.

• 대한화학회지
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• 제11권2호
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• pp.56-59
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• 1967

Ligand Exchange를 원리로 하여 Nickel Ion을 포함하고 있는 Chelating Resin인 dowex A-1을 써서 Elution Chromatography에 의하여 Amine의 혼합물을 분리하는 방법을 기술하였다. 이 실험에서 암모니아 수용액을 Eluent로 썼다. 이 방법은 특히 방향족아민의 분리에 효과 있음을 알게 되었다.