• Asian Journal of Atmospheric Environment
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• 제11권4호
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• pp.283-299
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• 2017

An analytical method using high-performance liquid chromatography (HPLC) with fluorescence (FL) detection was developed for simultaneously analyzing 10 polycyclic aromatic hydrocarbons (PAHs) and 18 nitro-derivatives of PAHs (NPAHs). The two-dimensional HPLC system consists of an on-line clean-up and reduction for NPAHs in the 1st dimension, and separation of the PAHs and the reduced NPAHs and their FL detection in the 2nd dimension after column-switching. To identify an ideal clean-up column for removing sample matrix that may interfere with detection of the analytes, the characteristics of 8 reversed-phase columns were evaluated. The nitrophenylethyl (NPE)-bonded silica column was selected because of its shorter elution band and larger retention factors of the analytes due to strong dipole-dipole interactions. The amino-substituted PAHs (reduced NPAHs), PAHs and deuterated internal standards were separated on polymeric octadecyl-bonded silica (ODS) columns and by dual-channel detection within 120 min including clean-up and reduction steps. The limits of detection were 0.1-9.2 pg per injection for PAHs and 0.1-140 pg per injection for NPAHs. For validation, the method was applied to analyze crude extracts of fine particulate matter ($PM_{2.5}$) samples and achieved good analytical precision and accuracy. Moreover, the standard reference material (SRM1649b, urban dust) was analyzed by this method and the observed concentrations of PAHs and NPAHs were similar to those in previous reports. Thus, the method developed here-in has the potential to become a standard HPLC-based method, especially for NPAHs.

• 대한환경공학회지
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• 제32권5호
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• pp.455-460
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• 2010

본 연구에서는 프탈레이트 화합물 측정 시 시료채취 및 분석과정 증에서 야기될 수 있는 공시료의 오염여부를 평가하고 clean-up 절차와 같은 적절한 개선 방안을 제시하였다. 실험도구 및 시료채취 매체에 대한 공시료를 평가한 결과 많은 종류의 실험기구 및 장치에서 DBP와 DEHP가 잔존하는 것으로 나타났다. 따라서 실험도구는 반드시 전처리하여 사용해야 하며, 이후 공시료 보정이 수반되어야 한다. 또한 본 연구에서 제시한 clean-up 방법을 통해 불순물이 많이 제거되었으며, GC/MS를 이용한 정성?정량분석에서 정도개선에 효과적인 것으로 나타났다.

• FOCUS: LIFE SCIENCE
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• 제1호
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• pp.1.1-1.4
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• 2024

This article provides comprehensive guidance on the maintenance, cleaning, regeneration, and storage of silica-based HPLC (High-Performance Liquid Chromatography) columns. The general considerations emphasize the importance of using in-line filters and guard cartridges to protect columns from blockage and irreversible sample adsorption. While these measures help, contamination by strongly adsorbed sample components can still occur over time, leading to an increase in back pressure, loss of efficiency, and other issues. To maximize column lifetime, especially with UHPLC (Ultra-High Performance Liquid Chromatography) columns, it is advisable to use ultra-pure solvents, freshly prepared aqueous mobile phases, and to filter all samples, standards, and mobile phases. Additionally, an in-line filter system and sample clean-up on dirty samples are recommended. However, in cases of irreversible compound adsorption or column voiding, regeneration may not be possible. The document also provides specific recommendations for column cleaning procedures, including the flushing procedures for various types of columns such as reversed phase, unbonded silica, bonded normal phase, anion exchange, cation exchange, and size exclusion columns for proteins. The flushing procedures involve using specific solvents in a series to clean and regenerate the columns. It is emphasized that the flow rate during flushing should not exceed the specified limit for the particular column, and the last solvent used should be compatible with the mobile phase. Furthermore, the article outlines the storage conditions for silica based HPLC columns, highlighting the impact of storage conditions on the column's lifetime. It is recommended to flush all buffers, salts, and ion-pairing reagents from the column before storage. The storage solvent should ideally match the one used in the initial column test chromatogram provided by the manufacturer, and column end plugs should be fitted to prevent solvent evaporation and drying out of the packing bed.

• 한국물환경학회지
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• 제22권5호
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• pp.879-886
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• 2006

The analytical methods of polychlorinated dibenzo-p-dioxins, polychlorinated dibenzofurans (PCDD/Fs) for water sample with extremely low concentration was developed to extract large volume and to improve fast chromatography for clean up. Semi-automated solid phase extraction (SPE) system and column coupling chromatography using elution pump was optimized and applied to each processes of treatment plant. Results of disk type SPE indicated that this system was applicable below 40 L of aqueous sample with a flow rate of 0.08 ~ 0.2 L/min. Average recoveries of SPE using labeled sampling spike of $^{37}Cl$-2,3,7,8-TCDD was 97%. Column coupling method resulted in reduced clean up time, solvent volume, increased average recoveries with constant elution rate. The combined methods were applied to the monitoring of drinking water treatment plant. Limits of detection (LOD) of each process were calculated. For example, LOD of raw and treated water ranged 0.094~0.968 pg/L and 0.028~0.364 pg/L, respectively. Combined methods of extraction and cleanup techniques provided fast analysis of PCDD/Fs with high accuracy and low LODs for water samples.

• 대한약학회:학술대회논문집
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• 대한약학회 2002년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2
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• pp.398.2-398.2
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• 2002

A column switching HPLC assay was developed to allow the separation and quantitation of cetirizine in human plasma by ultraviolet (UV) detection. Plasma samples were prepared by liquid-liquid extraction. After drying, the residue was reconstituted in 20 mM phosphate buffer (pH 2.8) containing 15% acetonitrile. The samples were initially injected onto a clean-up Capcell Pak MF C18 column. (50 mm $\times$ 4.6 mm I.D.), and the chromatographic region containing the peaks of interest was followed in an analytical C18 microcolumn (250 mm$\times$1.5 mm I. D.) via column switching device. (omitted)

• 대한약학회:학술대회논문집
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• 대한약학회 2002년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2
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• pp.397.1-397.1
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• 2002

A human immune globulin preparation (histobulin\ulcorner) are made to bind a small amount of histamine (0.15 $\mu$g) to the protein (12 mg) to increase the resistance of histamine susceptibility in the treatment of allergic diseases. Strict control of histamine content of the drug are required since intake of histamine might result in hypo- or hypertension. headache. or anaphylactic shock syndromes. HPLC analytical method with pre-column fluorescent derivatizalion after clean-up by solid-phase extraction (SPE) was developed. (omitted)

• 한국지하수토양환경학회지:지하수토양환경
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• 제17권4호
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• pp.63-72
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• 2012

The main objective of this study is to assess the compatibility between Korean ministry of environment (KME) standard and ISO (KS I ISO) standard for the determination of BTEX and TPH content in soil. We carried out comparison analysis for both methods using CRM and matrix spiked samples. In case of GC-MS analysis for BTEX, we got statistically (significance level: 0.05) the same results from KME standard (ES 07600.1) and ISO standard (KS I ISO 15009). However, it showed statistically (significance level: 0.05) different results when TPH was analyzed by KME standard (ES 07552.1) and ISO standard (KS I ISO 16703). To clarify the reason why both methods produced different results for TPH content, we also did some additional experiments in terms of differences in extraction, clean-up and target hydrocarbon range. Extraction with polar and non-polar compounds mixed solvent (acetone+n-heptane) of KS I ISO 16703 showed higher extraction efficiency than with only non polar solvent (dichloromethane) extraction of ES 07552.1 by about 9%. While column type clean-up of KS I ISO 16703 showed the reduction in TPH content between before and after clean-up, batch type of clean-up of ES 07552.1 did not show any changes in TPH content through clean-up process. The target hydrocarbon range of ES 07552.1 and KS I ISO 16703 is $C_8{\sim}C_{40}$ and $C_{10}{\sim}C_{40}$, respectively. From this point of view, kerosene and JP-8 contaminated soil showed higher RPD (relative producibility deviation) values between results by both method than that of lubricant or diesel contaminated soil. The higher content of hydrocarbon ($C_8{\sim}C_{10}$) in kerosene and JP-8 played an important role in increasing RPD values in addition to the effects caused by different solvents and clean-up method. Consequently, it was concluded that both methods (ES 07552.1 and KS I ISO 16703) were not compatible.

• 한국식품위생안전성학회지
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• 제5권3호
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• pp.159-164
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• 1990

To detect and quantitation residual antibiotics and antibacterial agents in meats, we performed a biological assay employing the three microorganisms Bacillus subtilis ATCC 6633, Micrococcus luteus ATCC 9341, and Bacillus cereus var. mycoides ATCC 11778 for the screening purpose and developed a Gas Chromatography-mass Spectrometry(GC/MS) analysis for the confirmation and quantiation. In the biological assay (paper disk method), three test solution are used depending on the character of the residual antibiotics and antibacterial agents, follow by a simple clean up procedure which includes homogenization with Mcilvaine buffer, defatting with includes homogenization with Mcilvaine buffer, defatting with hexane, extraction with chloroform, clean-up by Sep-Pak $C_{18}$ and Bakerbond SPE carboxylic acid column. The chloroform layer is used for the analysis of sulfa agents. macrolides antibiotics and antibacterial agents, Adsorbed materials in the Sep-Pak $C_{18}$ were also employed for th analysis of penicillins and tetracyclines. Effluents from the Sep-Pak $C_{18}$ were cleaned-up one more by Bakerbond 10 SPE COOH column and employed for the analysis of aminoglycosides. In the instrumental analysis by using the GC/MSD, residual antibiotics and antibacterial agent were quantitated by selected ion monitoring (SIM) mode after derivatization. A simultaneous analysis of six residual antibiotic and antibacterial agent such as oxytetracycline, penicillin, ampicillin, choliraphenicol and thiamphenicol was developed with simple cleanup procedures revealing good recovery and reproducibility. Also, simultaneous detection of macrolides antibiotics such as erythromycin, spiramycin, and oleandomycin was developed after acid hydrolysis due to their large molecular structures. Because of the high reproducibility and selectivity of these two methods, it is very desirable that the combination of the two methods be used in the bioassay for the screening of residual antibiotics and antibacterial agent and that GC/MSD analysis be used for the confirmation and quantitation.

• 청정기술
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• 제8권2호
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• pp.93-99
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• 2002

Adsorption dynamics for toluene and trichloroethylene with an isothermal fixed bed of activated carbon fiber were investigated. Equilibrium isotherms were measured by a static method for toluene and trichloroethylene onto activated carbon fiber at temperatures of 298, 323, and 348 K and pressure up to 3 kPa for toluene and 6 kPa for trichloroethylene, respectively. These results were correlated by the Toth equation. And dynamic experiments in an isothermal condition of 298 K were examined. Breakthrough curves reflected the effects of the experimental variables such as partial pressures for adsorbate and interstitial bulk velocities of gas flow. To present the column dynamics, a dynamic model based on the linear driving force (LDF) mass transfer model was applied.

• 한국수소및신에너지학회논문집
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• 제22권1호
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• pp.13-20
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• 2011

$SO_2$ has been absorbed and separated selectively by an ionic liquid from $SO_2/O_2$ mixture decomposed from sulfuric acid during the thermochemical SI cycle for the water splitting. In order to design and operate high pressure $SO_2/O_2$ separation system, the solubility of $SO_2$ in [EMIm]$EtSO_4$ (1-ethyl-3-methylimidazolium ethylsulfate) has been measured by Magnetic Suspension Balance at high pressure and temperature. Based on the measured solubility, a pressurized separation system was set up and operated. 194 L/h of $SO_2$($SO_2:O_2$=0.65:1) has been separated with 99.85% of $O_2$ at the vent of absorption tower, which is 22.7% of the theoretically ideal capacity of the system. This discrepancy results from the reduced contact between the gaseous $SO_2$ and the ionic liquid. Increased $SO_2$ supply, scale-up of the absorption column, and a faster ionic liquid circulation speed were suggested to improve the separation capacity.