• Mass Spectrometry Letters
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• 제5권1호
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• pp.30-33
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• 2014

A solid phase extraction (SPE) method was optimized for the quantitative analysis of perfluorooctanoic acid (PFOA) in serum using hydrophilic-lipophilic balance SPE and LC-MS/MS. Fetal bovine serums spiked with $^{13}C_8$-PFOA before or after SPE were used as test samples for evaluation of the SPE efficiency. Simultaneous evaluation of matrix effects and absolute SPE recovery for $^{13}C_8$-PFOA in serum using different sample pre-treatments and SPE conditions allowed optimization of SPE process efficiency with minimal matrix effect and decent SPE recovery. Introduction of protein precipitation as a sample pre-treatment procedure for serum samples before SPE generally decreased matrix effect in LC-MS/MS analysis and provided more stable recovery of PFOA.

• Toxicological Research
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• 제12권2호
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• pp.163-169
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• 1996

The focus of this study was to investigate the suitable analytical methods for measurement of sulfamerazine and its metabolite in shrimp hepatopancreas and tail tissue, in addition to the methods for the optimization of solid-phase extraction cartridge conditions and the elucidation of sulfamerazine concentrations in aqueous buffer using HPLC with UV and EC detectors. Compared with UV detector the EC detector appears to be 10 times more sensitive than that of the UV detector. After the shrimp was exposed to 10 ppm sulfamerazine, the accumulation levels of sulfamerazine and its metabolite in tail tissue, which is edible portion, were considerably lower than 0.1 ppm. The data indicate that sulfamerazine continues to be a candidate for use at levels of sulfamerazine concentration used in aquaculture of shrimp.

• 분석과학
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• 제30권4호
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• pp.174-181
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• 2017

Bio-liquid is a liquid by-product of the hydrothermal carbonization (HTC) reaction, converting wet biomass into solid hydrochar, bio-liquid, and bio-gas. Since bio-liquid contains various compounds, it requires efficient sampling method to extract the target compounds from bio-liquid. In this research, fatty acid methyl ester (FAME) in bio-liquid was extracted based on hollow fiber supported liquid phase microextraction (HF-LPME) and determined by Gas Chromatography-Flame Ionization Detector (GC-FID) and Gas Chromatography/Mass Spectrometry (GC/MS). The well-known major components of biodiesel, including methyl myristate, palmitate, methyl palmitoleate, methyl stearate, methyl oleate, and methyl linoleate had been selected as standard materials for FAME analysis using HF-LPME. Physicochemical properties of bio-liquid was measured that the acidity was 3.30 (${\pm}0.01$) and the moisture content was 100.84 (${\pm}3.02$)%. The optimization of HF-LPME method had been investigated by varying the experimental parameters such as extraction solvent, extraction time, stirring speed, and the length of HF at the fixed concentration of NaCl salt. As a result, optimal conditions of HF-LPME for FAMEs were; n-octanol for extraction solvent, 30 min for extraction time, 1200 rpm for stirring speed, 20 mm for the HF length, and 0.5 w/v% for the concentration of NaCl. Validation of HF-LPME was performed with limit of detection (LOD), limit of quantitation (LOQ), dynamic range, reproducibility, and recovery. The results obtained from this study indicated that HF-LPME was suitable for the preconcentration method and the quantitative analysis to characterize FAMEs in bio-liquid generated from food waste via HTC reaction.

• Advances in nano research
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• 제10권3호
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• pp.295-312
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• 2021

A new ionic liquid functionalized magnetic silica nanoparticle was synthesized and characterized and tested as an adsorbent. The adsorbent was used for magnetic solid phase extraction on ICP-MS method. Simultaneous determination of precious metal Au has been addressed. The method is simple and fast and has been applied to standard water and surface water analysis. A new method for separation/analysis of trace precious metal Au by Magnetron Solid Phase Extraction (MSPE) combined with ICP-MS. The element to be tested is rapidly adsorbed on CoFe2O4@SiO2@[BMIM]PF6 composite nano-adsorbent and eluted with thiourea. The method has a preconcentration factor of 9.5-fold. This method has been successfully applied to the determination of gold in actual water samples. Hydrophobic Ionic Liquids (ILs) 1-butyl-3-methylimidazole hexafluorophosphate ([BMIM]PF6) coated CoFe2O4@SiO2 nanoparticles with core-shell structure to prepare magnetic solid phase extraction agent (CoFe2O4@SiO2@ILs) and establish a new method of MSPE coupled with inductively coupled plasma mass spectrometry for separation/analysis of trace gold. The results showed that trace gold was adsorbed rapidly by CoFe2O4@SiO2@[BMIM]PF6 and eluanted by thiourea. Under the optimal conditions, preconcentration factor of the proposed method was 9.5-fold. The linear range, detection limit, correlation coefficient (R) and relative standard deviation (RSD) were found to be 0.01~1000.00 ng·mL-1, 0.001 ng·mL-1, 0.9990 and 3.4% (n = 11, c = 4.5 ng·mL-1). The CoFe2O4@SiO2 nanoparticles could be used repeatedly for 8 times. This proposed method has been successfully applied to the determination of trace gold in water samples.

• Bulletin of the Korean Chemical Society
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• 제34권9호
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• pp.2691-2696
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• 2013

The electronic cigarette (E-cigarette) is a battery-powered device that aerosolizes nicotine so that it is readily delivered into the respiratory tract. The analytical data regarding the substances present in E-cigarettes are very limited. The aim of this study was to measure the concentration of aldehydes-formaldehyde (FA), acetaldehyde (AA) and, acrolein (AL)-in 225 replacement liquid brands from 17 E-cigarette shops sold in the Republic of Korea by headspace solid-phase micro extraction and gas chromatography-mass spectrometry (HS-SPME GC-MS). The concentration range of FA and AA was 0.02-10.09 mg/L (mean = 2.16 mg/L, detected in 207 of 225 samples) and 0.10-15.63 mg/L (mean = 4.98 mg/L, detected in all samples), respectively. AL was not detected in any of 225 replacement liquids. FA and AA were originally present in almost all replacement liquids of electronic cigarettes.

• 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.401.3-402
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• 2002

Enalapril (ENP) maleate is effective drug for the treatment of renivascular hypertension and heart failure. ENP acts as inhibitor of the enzyme angiotensin-convertase (ACE-inhibitor) and metabolized to enalaprilat (ENPT), which is the active metabolite that is really responsible for the therapeutic action. In the present study, a sensitive and rapid liquid chromatography/ electrospray ion trap tandem mass spectrometry (LC/MS/MS) method combined with high-throughput solid phase extraction (SPE) has been developed and validated for the simultaneous quantitative determination of ENP and ENPT in human plasma. (omitted)

• Bulletin of the Korean Chemical Society
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• 제26권6호
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• pp.943-946
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• 2005

An effective spectrophotometric determination of palladium with 4-(2-pyridylazo)-resorcinol (PAR) using molten naphthalene as a diluent has been studied. A red complex of palladium with PAR is formed at 90 ${^{\circ}C}$. In the range of pH 9.0-11.0, the complex is quantitatively extracted into molten naphthalene. The organic phase is anhydrously dissolved in $CHCl_3$ to be determined spectrophotometrically at 520 nm against the reagent blank. Beer’s law is obeyed over the concentration range of 0.1-2 ${\mu}g{\cdot}mL^{-1}$. The molar absorptivity and Sandell’s sensitivity are 8.0 ${\times}\;10^5\;L{\cdot}mol^{-1}{\cdot}cm^{-}1\;and\;0.49\;{\mu}g{\cdot}cm^{-2}$ respectively. From the results of tolerance limits, it was found that there was no interferences were observed for most of the ions examined and those somewhat high interferences by Co(II), Fe(II) and Bi(III) could be effectively masked by EDTA.

• 분석과학
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• 제35권2호
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• pp.82-91
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• 2022

Grayanotoxin-contaminated honey exhibits toxicity. In this study, a reliable and sensitive liquid-chromatography-tandem-mass-spectrometric method (LC-MS/MS) was developed and validated for the quantitation of grayanotoxin I and grayanotoxin III in honey. The grayanotoxins were extracted from honey via solid phase extraction and separated on a biphenyl column with a mobile phase consisting of 0.5 % acetic acid in water and methanol. Mass spectrometric detection was performed in the multiple-reaction monitoring mode with positive electrospray ionization. The calibration curve covered the range 0.25 to 100 ㎍/g. The intra- and inter-day deviations were less than 10.6 %, and the accuracy was between 94.3 and 114.0 %. The validated method was successfully applied to the determination of grayanotoxins in mad honey from Nepal. The concentrations of grayanotoxin I and grayanotoxin III in 33 out of 60 mad honey samples were 0.75 - 64.86 ㎍/g and 0.25 - 63.99 ㎍/g, respectively. The method established herein would help in preventing and confirming grayanotoxin poisoning.

• Mass Spectrometry Letters
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• 제8권1호
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• pp.18-22
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• 2017

Products containing any one or more of 26 fragrance allergens likely to cause contact allergies, are required under the 2008 domestic cosmetic law to be labeled when their concentrations exceed a certain range. This study focuses on the comparison and development of analytical methods based on headspace-solid phase micro extraction (HS-SPME) and liquid-liquid extraction (LLE) methods followed by GC-MS/MS for 24 of the fragrance allergens excepting for two natural materials in water samples. Using the developed HS-SPME method, 15 of the 24 fragrance allergens were analyzed and 9 compounds which have relatively low $logK_{OW}$ values (below about 2.5) were not extracted, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9969 or more, and the method detection limits (MDL) and the limits of quantification (LOQ) were $0.078{\sim}0.582{\mu}g/L$ and $0.261{\sim}1.940{\mu}g/L$, respectively. In the case of using the optimized LLE method, all 24 fragrance allergens were analyzed, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9957 or more, MDL and LOQ were $0.020{\sim}0.138{\mu}g/L$ and $0.065{\sim}0.440{\mu}g/L$, respectively.

• 한국환경과학회지
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• 제19권3호
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• pp.379-387
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• 2010

Sediments of Little Scioto (LS) River in Ohio was contaminated by poor disposal of creosote from Baker Wood Creosoting Facility. Among the primary compounds of creosote, Polycyclic Aromatic Hydrocarbons (PAHs) are the most common ingredient PAHs are known for toxic, carcinogenic and mutagenic compounds. There are many difficulties to remove the PAHs in nature environment because their characteristics are having a less water-solubility, volatile and low mobility properties as increasing the molecular weight. The generation of hydroxyl radicals (${\cdot}OH$) and hydrogen peroxide ($H_2O_2$) forms as well as high temperature (5000 K) and pressure (1000 atm) by a physico-chemical effects of ultrasound during a cavitation collapse can promote the degradation and desorption of PAHs in sediment And it can also produces shock wave and microjets which are able to change the size and surface of particle in solid-liquid system as one of physical effects. Therefore, we explored to understand the role of particle size, the effect of elimination for PAHs concentration by ultrasound and optimize the conditions for ultrasonic treatment. The condition of various size of particles (> $150{\mu}m$, < $150{\mu}m$) and solid-liquid ratio (12.5g/L, 25g/L) for the treatment was considered and ultrasonic power (430 W/L) with liquid - hexane extraction and microwave extraction method were applied after ultrasound treatment.