• Mass Spectrometry Letters
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• v.13 no.4
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• pp.158-165
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• 2022

Many therapeutic class drugs such as beta-blocker, corticosteroids, NSAIDs, etc are prohibited substances in the horse racing industry. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) technology makes it possible to isolate drugs from interference, enables various drug analyses in complex biological samples due to its sensitive sensitivity, and has been successfully applied to doping control. In this paper, we describe a rapid and sensitive method based on solid-phase extraction (SPE) using solid phase cartridge and LC-MS/MS to screen for different class's 35 drug targets in equine plasma. Plasma samples were pretreated by SPE with the NEXUS cartridge consisted non-polar carbon resin and minimum buffer solvent. Chromatographic separation of the analytes was performed on ACQUITY HSS C18 column (2.1 × 150 mm, 1.8 ㎛). The elution gradient was conducted with 5 mM ammonium formate (pH 3.0) in distilled water and 0.1% formic acid in acetonitrile at a flow rate of 0.25 mL/min. The selected reaction monitoring (SRM) mode was used for drug screening with multiple transitions in the positive ionization mode. The specificity, limit of detection, recovery, and stability was evaluated for validation. The method was found to be sensitive and reproducible for drug screening. The method was applied to plasma sample analysis for the proficiency test from the Association of Racing Chemist.

• Analytical Science and Technology
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• v.36 no.2
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• pp.89-98
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• 2023

Analytical methods for detecting atranol, chloroatranol, evernic acid, (+)-usnic acid, and atranorin in sanitary napkins and mouthwashes were developed using ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). UHPLC-MS/MS conditions were optimized for rapid, sensitive, and simultaneous analysis of the five allergenic compounds. The methods were validated by assessing their specificity, matrix effects, limit of detection (LOD), limit of quantification (LOQ), linearity, accuracy, and precision. Good linearity was achieved with a determination coefficient of ≥0.99. The LOD and LOQ were 2.1-9.8 and 6.4-29.6 ng/g for sanitary napkins and 0.29-0.48 and 0.87-1.45 ng/mL for mouthwashes, respectively. The accuracy and precision were within an acceptable range according to the criteria reported in the European SANTE/11813/2017 guidelines (70-120 % recovery, <20 % relative standard deviation). Therefore, these methods can be used to analyze atranol, chloroatranol, evernic acid, (+)-usnic acid, and atranorin in sanitary napkins and mouthwashes.

• Korean Journal of Pharmacognosy
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• v.54 no.1
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• pp.38-43
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• 2023

A simple and accurate assay was developed for the quantitative analysis of 1-deoxynojirimycin (1-DNJ) derived from the silkworm (Bombyx mori). Normal-phase high-performance liquid chromatography coupled with an evaporative light scattering detector (HPLC-ELSD) and a hydrophilic interaction liquid chromatography column was used. Various parameters were applied to optimize the analysis method. The limits of detection and quantification of 1-DNJ were 2.97 × 10^-3 and 9.00 × 10^-3 mg/mL, respectively. The calibration curve showed good linearity results. The concentration range and the r² value were 0.0625-1.0 mg/mL and 0.9997, respectively. The accuracy test demonstrated a significantly high recovery rate (89.95-103.22%). The relative standard deviation was ≤ 1.00%. Thus, a method for the accurate identification and quantitative analysis of 1-DNJ in silkworms was developed. Moreover, in this procedure, the process of derivatization of 1-DNJ, which was required in previous experiments, could be eliminated. This technique may be actively utilized for the development of pharmaceuticals and health functional foods using 1-DNJ.

• Journal of Applied Biological Chemistry
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• v.66
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• pp.67-72
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• 2023

A simple and accurate method was developed for the quantitative analysis of oleanonic acid (OA) from mastic gum. The analysis was carried out using reverse-phase high-performance liquid chromatography combined with a photodiode array detector (HPLC/PDA). Our optimized method was validated by measuring various parameters, using an INNO C18 column fitted with a gradient elution system. The results revealed limits of detection and quantification of 0.34 and 1.042 ㎍/mL, respectively. The OA calibration curve exhibited excellent linearity over the concentration range of 0.0625 to 2.0 mg/mL, with r² =0.9996. Accuracy tests revealed a high recovery rate of 99.44-103.66%, with precision values below 0.15%. These results suggest that the present analytical method can identify and quantify OA in mastic gum with high precision. The HPLC approach developed in this study might be applied to routine analyses and large-scale extraction procedures for OA content quantification.

• Toxicological Research
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• v.31 no.3
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• pp.255-264
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• 2015

Heterocyclic amines (HCAs) and acrylamide are unintended hazardous substances generated by heating or processing of foods and are known as carcinogenic and mutagenic agents by the animal experiments. A simple method was established for a rapid and accurate determination of 12 types of HCAs (IQ, MeIQ, Glu-P-1, Glu-P-2, MeIQx, Trp-P-1, Trp-P-2, PhIP, $A{\alpha}C$, $MeA{\alpha}C$, Harman and Norharman) and acrylamide in three food matrices (non-fat liquid, non-fat solid and fat solid) by isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS). In every sample, a mixture of internal standards including $IQ-d_3$, $MeIQx-d_3$, $PhIP-d_3$, $Trp-P-2-^{13}C_2-^{15}N$ and $MeA{\alpha}C-d_3$ was spiked for quantification of HCAs and $^{13}C_3$-acrylamide was also spiked for the analysis of acrylamide. HCAs and acrylamide in sample were extracted with acetonitrile and water, respectively, and then two solid-phase extraction cartridges, ChemElut: HLB for HCAs and Accucat: HLB for acrylamide, were used for efficiently removing interferences such as pigment, lipid, polar, nonpolar and ionic compounds. Established method was validated in terms of recovery, accuracy, precision, limit of detection, limit of quantitation, and linearity. This method showed good precision (RSD < 20%), accuracy (71.8~119.1%) and recovery (66.0~118.9%). The detection limits were < 3.1 ng/g for all analytes. The correlation coefficients for all the HCAs and acrylamide were > 0.995, showing excellent linearity. These methods for the detection of HCAs and acrylamide by LC-MS/MS were applied to real samples and were successfully used for quantitative monitoring in the total diet study and this can be applied to risk assessment in various food matrices.

• Resources Recycling
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• v.28 no.2
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• pp.46-53
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• 2019

In this study, the extraction and reduction behavior of platinum group metals in a non-aqueous solvent based on ionic liquids was investigated in order to confirm a new extraction technology of platinum group metals. Platinum was selectively extracted using an ionic liquid $[C_4mim]PF_6$ from a mixed solution of $PdCl_2$, $PtCl_4$ and $RhCl_3$ dissolved with concentration ratio of 10:1:0.5 M. After stripping of the metals by 1 M $HNO_3$ solution, the platinum was preferentially reduced by aqueous electrolysis on gold electrode at -0.8 V (vs. Pt-QRE). The residual palladium and rhodium were transferred to ionic liquid of $[C_4mim]Cl$. The metallic palladium and rhodium could be sequentially reduced on gold and STS304 as working electrodes by non-aqueous electrolysis, respectively.

• Analytical Science and Technology
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• v.22 no.3
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• pp.191-200
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• 2009

The aim of this study was to evaluate and establish of emission test method for liquid phase building materials such as paint, adhesive, sealant by emission cell. A small-scale emission chamber and emission cell were used to evaluate emission of TVOC from paint, adhesive, sealant. The quantity of TVOC emission were measured by a gas chromatography/mass spectrometry (GC/MS). Background concentration of TVOC was below $10{\mu}g/m^3$ in the emission chamber and cell. Air tightness and recovery in chamber and cell showed good results. The recovery of thermal desorber for toluene and n-dodecane were about 120%. The repeatability of response factor and retention time in GC/MS below 30%. The method detection limit of VOCs ranged 0.04~8.82 ng. The concentration of TVOC emission using emission cell was 1.35~1.41 times higher than emission chamber. The correlation of TVOC emission using chamber and cell method was significantly high (r=0.91~0.97).

• Proceedings of the Korean Vacuum Society Conference
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• 2016.02a
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• pp.267.1-267.1
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• 2016

본 연구에서는 nematic 액정의 종류 중 하나인 5CB (4-Cyano-4'-pentylbiphenyl) 물질을 박막 트랜지스터 (TFT)의 passivation 층으로 사용했을 때 그 전기적 특성향상을 확인하였다. RF-magnetron sputtering법으로 증착된 비정질 InGaZnO 박막을 활성층으로 사용한 TFT를 제작하여 그 활성층 위에 drop형식으로 passivation 하였다. 그 결과, drain current (I_DS)가 약 10배 정도 증가하고, linear region(V_D=0.5V)에서 mobility와 subthreshold slope(SS)이 각각 6.7에서 12.2, 0.3에서 0.2로 향상되는 것이 보였다. 이것은 gate bias가 인가되었을 때 freedericksz 전이를 통한 액정의 배향과 이때 형성된 dipole 형성에 의한 것으로 보이며, 이러한 LC의 배향은 편광현미경을 통하여 표면과 수직으로 배향한다는 사실을 확인 할 수 있었고 이 LC-passivation된 a-IGZO TFT의 전기적 특성의 향상에 대한 mechanism을 제시하였다. 그리고 배향한 LC가 가지는 dipole에 의해 bias stress 상황에서 독특한 electron trapping과 recovery의 증폭효과가 나타났다. V_G=+20V의 positive gate bias stress를 1000s동안 가했을 때, passivation되지 않은 a-IGZO TFT의 경우 +4V의 threshold voltage shift(${\Delta}V$_TH)가 발생되었고, 바로 -20V의 negative gate bias를 30s간 가해주었을 때 -2.5V의 ${\Delta}V$_TH가 발생하였다. 반면 LC-passivation된 a-IGZO TFT의 경우 각각 +5V와 -4V의 ${\Delta}V$_TH로 더 큰 변화를 가져왔다. 이러한 LC에 의한 electron trapping/recovery 증폭효과에 대한 model을 제시하였다.

• Economic and Environmental Geology
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• v.38 no.6 s.175
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• pp.657-662
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• 2005

Extractions fro fertilizer and soil samples were performed to yield the operationally defined fractions 'soluble' chromate (extractable with $NH_4NO_3$), 'exchangeable' chromate (extractable with phosphate buffer pH 7.2), and these results were compared with the data obtained by extractions with ammonium sulfate, borate buffer pH 7.2, saturated borax pH 9.6, and polyphosphate (Graham's salt). In order to maintain the pH of extractant solution about constant, the concentration of extractant buffer had to be raised to at least 0.5 M. The results strongly depended on the kind of extractant, and the solid: liquid ratio. For most of the samples investigated, the extraction efficiency increased in the order borate-sulfate-nitrate-phosphate. Whereas the recovery of $K_2CrO_4\;and\;CaCrO_4$ added to the samples of basic slags prior to the extraction was about complete, the recovery of added $PbCrO_4$ was highly variable. In soil extracts, the color reaction was interfered from co-extracted humics, which react with the chromate in weak acid solution during the time period necessary for color reaction (1 hour). However, this problem can be overcome by standard addition and subtraction of the color of the extractant solution. In soil extract of about pH < 7, organic material reduced chromate during the extraction period also, and standard addition of soluble chromate is recommended to prove recovery and the stability of chromate in the samples. In admixtures of soils and basic slags, results for hexavalent chromium were lower than from the mere basic slags. This effect was more pronounced in phosphate than in nitrate extracts. As a proficiency test, samples low in organic carbon from contaminated sites in Hungary were tested. The results from $NH_4NO_3$ extracts satisfactorily matched the results of the Hungarian labs obtained from $CalCl_2$ extractants.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.12 no.3
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• pp.1473-1478
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• 2011

In this study, simulation and optimization works for a demethanizer column have been performed to obtain ethane and heavier products from a pretreated natural gas stream. Pretreated natural gas feed stream is partially condensed after being precooled by exchanging heat with demethanizer top vapor stream and by using an external refrigeration cycle with a propane refrigerant. Vapor stream is furtherly cooled and partially condensed through a turbo-expander and the power generated from the expansion of turbo-expander was delivered to the compressor for the residue gas compression. Liquid stream is being cooled by Joule-Thomson expansion valve and is fed to the middle section of the demethanizer. Ethane recovery percent for feed natural gas was set to 75% and methane to ethane molar ratio was fixed as 0.015. Propane refrigeration heat duty was reduced by splitting the feed stream and to exchange heat with side reboiler.