• Journal of the Korean Chemical Society
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• v.61 no.2
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• pp.51-56
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• 2017

N-nitrosamines are the nitroso compounds which are produced by nitrosation reactions of the secondary amine and nitrite under acidic conditions. Approximately 300 species of N-nitrosamine have been tested for carcinogenicity in laboratory experiments, with 90% of them demonstrated carcinogenic effects different animal species, including higher primates. In 1978, IARC classified NDMA and NDEA as Group 2A, and NDPA, NDBA, NPIP, NPYR and NMOR as Group 2B. In this study, we established pretreatment and analytical method for N-nitrosamines (NDMA, NDEA, NMEA, NDPA, NDBA, NPIP, NPYR and NMOR) in human urine for biological monitoring of N-nitrosamines. The analytes were extracted using solid phase extraction (SPE), then quantitative analysis was performed by LC-(APCI)-MS/MS. The accuracies of the established method were between 85.8~108.7% and precisions were lower than 20%. The limit of detection (LOD) were between 0.0002 (NDBA) and 0.0793 (NDMA) ng/ml. The linearity obtained was satisfying for the 8 N-nitrosamines, with a coefficient of determination ($r^2$) higher than 0.999. The mean concentrations of N-nitrosamines in the urine were 2.645 mg/g creatinine for NDMA, 0.067 mg/g creatinine for NDEA, 0.009 mg/g creatinine for NMEA, 0.011 mg/g creatinine for NDBA, 0.271 mg/g creatinine for NPIP and 0.413 mg/g creatinine for NPYR. NDPA and NMOR were not detected. It can be used as a instrumental methodology for evaluation and risk assessment of human exposure to N-nitrosamines for the further research.

• Analytical Science and Technology
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• v.23 no.2
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• pp.119-127
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• 2010

An effective method for the simultaneous analysis of ${\beta}$-lactams from surface water was established. After solid-phase extraction with HLB (Hydrophilic Lipohilic Balance) cartridge at pH 2, seven ${\beta}$-lactams (amoxicillin, ampicillin, penicillin G, cefaclor, cefadroxil, cefatrizine and cephradine) were determined using LC/ESI-MS/MS. In this newly established method, correlation coefficients ($r^2$) of calibration curves for seven ${\beta}$-lactams in blank surface water appeared to be 0.9911~0.9995 in the concentration range of 0.01~1.0 ng/mL. The limits of detection (LODs) and the limits of quantificaiton (LOQs) in spiked surface water were shown to be 0.0003~0.0234 ng/mL and 0.0046~0.0778 ng/mL, respectively. The developed method is believed to serve as a rapid and reliable method for the qualitative and quantitative analysis of residual ${\beta}$-lactam antibiotics from aquatic environment.

• Analytical Science and Technology
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• v.21 no.1
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• pp.41-47
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• 2008

Although liquid-liquid extraction (LLE) method has been used routinely for the analysis of amphetamine-like drugs (amphetamine; AP, methamphetamine; MA, 3,4-methylenedioxyamphetamine; MDA, 3,4-methylenedioxymethamphetamine; MDMA, 3,4-methylenedioxyethylamphetamine; MDEA), a solid-phase extraction (SPE) method, which can be automated, was applied for the simultaneous determination by GC/MS in human urine. Urine samples (3 mL) and 0.1 M phosphate buffer (1 mL, pH 7.0) were extracted by an automated SPE system. The eluent was evaporated, derivatized with trifluoroacetic anhydride (TFAA), and analyzed by GC/MS. The calibration curves was linear with correlation coefficient ($r^2$) above 0.994 in the ranges of 34.0 (AP), 28.0 (MDA)~1000.0 ng/mL for AP, MDA, and 50.0~2000.0 ng/mL for MA, MDMA, and MDEA. The limits of detection ranged from 4.0 to 10.0 ng/mL, and the limits of quantitation ranged from 12.0 to 34.0 ng/mL. The relative recoveries were 93.5~107.7 %. The precisions and accuracies were 1.9~14.8 % and -8.7~14.8 %, respectively. The present method was successfully applied to identify the MA or Ecstasy (MDMA) abusers in exact as well as rapid.

• Analytical Science and Technology
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• v.16 no.2
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• pp.102-109
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• 2003

Microwave digestion and solid-state extraction were studied for determination of trace aluminum{Al(III)} in human urine samples. A mixed acid of nitric acid and hydrogen peroxide was added to urine samples, organic materials were destructed in a home microwave oven and dried in a drying oven. The dried residues were dissolved in a sulfuric acid solution. The solution was eluted through a XAD-4 resin column adsorbed with 8-hydroxyquinoline(Oxine, HQ). Al(III)-8-hydroxyquinolinate complex was formed in the column and eluted with 0.5 M nitric acid solution. The Al(III) eluted was determined by graphite atomic absorption spectrophotometry. Various experimental conditions of followings were investigated for the optimization : the type of acid to dissolve the residues, the amount of HQ adsorbed on the resin, the pH of sample solutions, the type and concentration of acid to elute the complex from column and so on. The contents of Al(III) in real samples were determinated by a calibration curve method. The recovery in standard spiked samples was 94~101% and the detection limit of this procedure was 0.05 ng/mL.

• Journal of Soil and Groundwater Environment
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• v.12 no.5
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• pp.73-85
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• 2007

In this study, the experiment of solid-phase microextraction (SPME) technique using GC/FID was conducted as a possible alternative to liquid-liquid extraction for the analysis of EGBE, DGBE, DBM and TGME in water, and also, an optimization condition of trace analysis for disel oxygenates including EGBE by the design of experiment (DOE) was described. Experiments used a fractional factorial design method followed by central composite design allowing optimization of a number of factors as well as statistical analysis of the results. The response surface analysis showed that the extraction efficiency could be represented by a second-order polynomial equation in which the salts concentration, extraction temperature, extraction time and sonication time are the major influences. Using DOE method, a new datadependent method was developed to improve the quantity of confidently analyzed disel oxygenates in water samples.

• Analytical Science and Technology
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• v.27 no.2
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• pp.92-99
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• 2014

Interferences were removed using anion exchange solid phase extraction (AE SPE) in quantification of selenoproteins in Korean human blood serum with affinity high performance liquid chromatography (AF HPLC)-inductively coupled plasma/mass spectrometry (ICP/MS). The average selenium level obtained for healthy Koreans was $94.3{\pm}2.3ngg^{-1}$ using isotope dilution method. AE SPE was coupled to AF column to separate 3 selenoproteins, glutathione peroxidase GPx, selenoprotein SelP, and selenoalbumin SeAlb. Post column isotope dilution was employed to quantify the proteins. The certified reference material of human blood serum BCR-637 was analyzed to give total selenoprotein concentration of $85.4{\pm}3.4ngg^{-1}$, which agreed well with the reference value of $81{\pm}7ngg^{-1}$. The pooled concentration of GPx, SelP, and SeAlb from healthy Koreans (n=20) was $12.1{\pm}1.4ngg^{-1}$, $57.2{\pm}2.0ngg^{-1}$, and $20.0{\pm}1.9ngg^{-1}$, respectively. The sum of selenoproteins is $89.3ngg^{-1}$, which is about the same as the total selenium concentration of $94.3ngg^{-1}$. The fact suggests that selenium in blood serum is mostly consisted of selenoproteins. After the removal of interference, GPx showed a significant decrease (more than 50%) from $25.0ngg^{-1}$ to $12.1ngg^{-1}$. It was identified that the interference in blood serum was mostly from GPx and the use of AE SPE was proven to be efficient in eliminating Cl and Br that cause interference to GPx.

• Journal of the Korean Chemical Society
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• v.38 no.9
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• pp.640-652
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• 1994

This work is undertaken to determine alcohol homologues so-called fusel oil that may be present in the Korean folk sojues (distilled liquor) made from grains and to describe sample preparation and analytical method by GC-FID-MS. Solid phase extraction method for sample preparation by using porous styrene divinyl benzene polymer (Porapak Q) was compared with steam distillation and solvent extraction method. Retention behaviors of homologous series of alcohols were also studied. Log values of retention time, molecular weight, boiling point, and capacity factor of alcohols showed linear correlations to the carbon number of an alcohol, to the oven temperature, and to the dielectric constant. Components such as methyl alcohol, n-propyl alcohol, isobutyl alcohol, isopentyl alcohol, and phenethyl alcohol have been identified. The more amount of isopentyl alcohol than other alcohols are contained in the Korean folk sojues, while that of n-propyl alcohol are contained in Chinese kaoliangchiew. Degree of similarity or dissimilarity and classification of the individual samples were discussed using multivariate statistical analysis(principal components analysis) based on GC data.

• Journal of the Korean Chemical Society
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• v.34 no.4
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• pp.352-359
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• 1990

An effecient gas chromatographic method is described to be used routinely for the rapid profiling and identification of biochemically important organic acids. It involves the solid-phase extraction of organic acids from aqueous samples using Chromosorb P as the solid sorbent and diethyl ether as the eluting solvent, with subsequent triethylamine treatment. The resulting triethylammonium salts of acids were directly converted to volatile tert-butyldimethylsiyl derivatives, which were simultaneously analyzed by two capillary columns of different polarity, DB-5 and DB-1701, under the identical temperature programming condition. The retention index (RI) and area ratio (AR) values of each peak measured on DB-5 and DB-1701 enabled rapid identification of acids by computer RI library search and AR comparison. The application of the present method to the organic acid profiling of various complex samples is demonstrated.

• Analytical Science and Technology
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• v.23 no.6
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• pp.524-530
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• 2010

Chloramphenicol is one of the most effective antibiotics for treatment of food-producing animals for typhoid fever. However, it has been reported that it caused severe side effects such as aplastic anemia in human, therefore the use of chloramphenicol for food-producing animal is prohibited by European Union and other countries. In this study, the analytical method using isotope dilution liquid chromatography-mass spectrometry (ID-LC/MS) was established for accurate determination of chloramphenicol in meat. Chloramphenicol was extracted with ethylacetate from porcine and solid phase extraction cartridge was used for enhancing the recovery. The residue of chloramphenicol in porcine was analyzed using the liquid chromatography mass spectrometer (LC/MS) interfaced with electrospray ionization source. Analysis was performed in negative mode with selected reaction mornitoring mode at m/z 321${\rightarrow}$257 of $[M-H]^-$ ${\rightarrow}$ $[M-H-(HCOCl)]^-$ and m/z 326 ${\rightarrow}$ 262 channels for its isotope. The established method was tested using fortified samples at the level of 0.2 1, 10, $25\;{\mu}g$/kg and analytical results agreed with the gravimetrically fortified values within their uncertainties. This method was validated by analyzing a certified reference material, BCR 445, from IRMM (Institute for Reference Materials and Measurement). Our measurement values agreed with the certified value within their uncertainties. The uncertainty of our measured value was much lower than that the certified value from IRMM.

• Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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• 2005.04a
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• pp.195-198
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• 2005

A solid-phase microextraction and gas chromatography-mass spectrometry for the extraction and analysis of methyl-tert-butyl ether has been described. methyl-tert-butyl ether was extracted from aqueous solution using SPME fiber coated polydimethylsiloxane and analysed by GC-MS with capillary column. Extraction parameters and chromatographic separation conditions were optimized. The applied method represented good analytical performance in terms of precision (3-8%, RSD) and accuracy(93-102%, mean recovery) with a method detection limit of 0.03 ppb.