• YAKHAK HOEJI
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• v.60 no.3
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• pp.112-117
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• 2016

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of caffeine in forensic aqueous sample. The centrifuged sample ($100{\mu}l$) was diluted 50-fold with distilled water. The diluted sample ($400{\mu}l$) was then diluted further with $200{\mu}l$ of 0.1% formic acid solution and $400{\mu}l$ of acetonitrile containing 500 ng of caffeine-(3-methyl-$^{13}C_3$) prior to LC-MS/MS analysis. The mobile phase was composed of 0.1% formic acid in distilled water (A) and acetonitrile (B). Chromatographic separation was performed by using a Zorbax SB-C18 ($100mm{\times}2.1mm$ i.d., $3.5{\mu}m$) column and caffeine was eluted within 1.1 min. Linear least-squares regression with a 1/x weighting factor was used to generate a calibration curve with the coefficients of determination ($r^2=0.9983$). The lower limit of quantification was $25ng/ml$ for the analyte. The process efficiency was 98.6~100.1%. Intra- and inter-day precisions were not more than 2.1% and 1.7%, while intra- and inter-day accuracies were ranged from -6.8 to 4.5%, respectively. The suitability of the method was examined by analyzing unknown forensic aqueous samples.

• Bulletin of the Korean Chemical Society
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• v.25 no.8
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• pp.1133-1136
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• 2004

The need for highly reliable methods for the determination of trace metals is recognized in analytical chemistry and environmental science. A method based on the cloud-point extraction (CPE) technique for the trace analysis of Pb and Cu in water samples is described in this study. The analytes in the initial aqueous solution are complexed with pyrogallol, and 0.1%(w/v) Triton X-114 is added as surfactant. Following phase separation at $50^{\circ}C$, based on the cloud point of the mixture and dilution of the surfactant-rich phase with acidified methanolic solution, the enriched analytes are determined by flame atomic absorption spectrometry. After optimization of the complexation and extraction conditions, the enrichment factors of Pb and Cu were found to be 72 and 85, respectively. Under optimum conditions, the preconcentration of 60 mL of samples in the presence of 0.1%(w/v) Triton X-114 permitted the detection of 0.4 ${\mu}gL^{?1}$ of Pb and 0.05 ${\mu}gL^{?1}$ of Cu. The proposed method was applied successfully to the determination of Pb and Cu in water samples.

• Analytical Science and Technology
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• v.36 no.4
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• pp.152-160
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• 2023

Adenosine and cordycepin are bioactive compounds with health benefits. Therefore, both substances are often used to assess the quality of Cordyceps products. Optimization and validation of the HPLC/DAD method for determining two nucleosides were studied. The samples were prepared using an ultrasound-assisted extraction (ultrasonic bath). The result was optimal conditions for aqueous extraction, an extraction time of 35 min, and an extraction temperature of 40 ℃. The Chromatographic separation was achieved using a reverse phase column (InfinityLab Poroshell 120 EC-C18, 4.6 × 250 mm, 2.7 ㎛) at 30 ℃ with a mobile phase gradient elution of water and methanol at a flow rate of 0.7 mL/min. The eluents were monitored via a diode array detector at 260 nm. Two nucleosides were separated by less than 12 min after injection. The developed method was found to be excellent linear (r² > 0.9999), accurate (% recovery 95.34-98.51), and precise (% relative standard deviation < 2.0). The limit of detection (LOD) and quantification (LOQ) were 0.45 and 1.38 mg/mL for adenosine and 0.47 and 1.43 mg/mL for cordycepin, respectively. This method was satisfactory for simultaneously quantitating two nucleoside contents, which were used to evaluate Cordyceps products.

• Journal of Ginseng Research
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• v.40 no.3
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• pp.220-228
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• 2016

Background: Among the various ginseng strains, Shizhu ginseng is endemic to China, mainly distributed in Kuandian Manchu Autonomous County (Liaoning Province, China); however, not much is known about the compounds (especially saponins) in Shizhu ginseng. Methods: A rapid, sensitive, and reliable ultra-high performance liquid chromatography coupled with MS/MS (UHPLC-MS/MS) method was developed to separate and identify saponins in Shizhu ginseng. Results: The separation was carried out on a Waters ACQUITY UPLC BEH $C_{18}$ column ($100mm{\times}2.1mm$, $1.7{\mu}m$) with acetonitrile and 0.1% formic acid aqueous solution as the mobile phase under a gradient elution at $40^{\circ}C$. The detection was performed on a Micromass Quattro Micro API mass spectrometer equipped with electrospray ionization source in both positive and negative modes. Under the optimized conditions, a total of 31 saponins were identified or tentatively characterized by comparing retention time and MS data with related literatures and reference substances. Conclusion: The developed UHPLC-MS/MS method was suitable for identifying and characterizing the chemical constituents in Shizhu ginseng, which provided a helpful chemical basis for further research on Shizhu ginseng.

• Applied Chemistry for Engineering
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• v.9 no.7
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• pp.968-973
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• 1998

The critical micelle concentrations($CMC^*$) of the mixed surfactant systems of cationic surfactant cetylpyridinium chloride(CPC) and nonionic surfactant Triton X-100(TX-100) in aqueous solutions of salts(KCl and $Na_2CO_3$) and isomeric butanols(tert-butanol, iso-butanol and n-butanol) were determined by UV spectroscopy method. The various thermodynamic values in aqueous solutions of salts and isomeric butanols were compared with the values in pure water, calculated by means of the equation derived from the pseudo-phase separation model. Thermodynamic parameters($X_1$, $\beta$, ${\gamma}i$, $ai^M$, $C_i$ and ${\Delta}H_{mix}$) were found to have great effects of salts and isomeric butanols on the mixed micellization of CPC/TX-100 mixtures, and also in good agreements with the nonideal mixed micelle model. They showed all negative deviations from the ideal mixed micellar behavior.

• Applied Chemistry for Engineering
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• v.8 no.6
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• pp.1006-1013
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• 1997

This study was carried out to elucidate the chemical characteristics of mutual separation for Am and Eu, which were selected as a stand-in from minor actinide and rare earth elements, by solvent extraction with di-(2-ethylhexyl)phosphoric acid containing zirconium at batch system. As results, 92.3% of Am and 99.1% of Eu were coextracted with 1M DEHPA/n-dodecane containing zirconium (Zr $concentration=8.7g/{\ell}$) at 0.5M $HNO_3$ in the extraction step. The extraction yields of Am and Eu were proportionally increased with the concentration of Zr in Zr salt of 1M DEHPA/n-dodecane having the synergistic effect. In the lst stripping step for the selective separation of Am, 38.1% of Am and 3% of Eu were stripped with the mixed solution of 0.05M DTPA and 1M lactic acid adjusted pH of 3.0. At that time, the separation factor calculated from the distribution coefficients of Am and Eu was 14.2. In the 2nd Stipping step to remove the Eu remained the organic phase after the lst stripping step, 94.4% 0f Eu was stripped into aqueous phase with 6M $HNO_3$.

• Membrane and Water Treatment
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• v.13 no.4
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• pp.201-208
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• 2022

Emulsion Liquid Membrane (ELM) is a prominent technique for the separation of heavy metal ions from wastewater due to the fast extraction and is a single-stage operation of stripping-extraction. The selection of the components (Surfactant and Carrier) of ELM is a very significant step for its preparation. In the ELM technique, the primary water- in-oil (W/O) emulsion is emulsified in water to produce water-in-oil-in-water (W/O/W) emulsion. The water in oil emulsion was prepared by mixing the membrane phase and internal phase. To prepare the membrane phase, the extractant D2EHPA (di-2-ethylhexylphosphoric acid) was used as a mobile carrier, Span-80 as a surfactant, and Paraffin as a diluent. Moreover, the internal (receiving) phase was prepared by dissolving sulphuric acid in water. Di-(2- ethylhexyl) phosphoric acid such as surfactant concentration, carrier concentration, sulphuric acid concentration in the receiving (internal) phase, agitation time (emulsion phase and feed phase), the volume ratio of the membrane phase to the receiving phase, the volume ratio of the external feed phase to the primary water-in-oil emulsion and pH of feed were studied on the percentage extraction of metal ions at 20℃. The results show that it is possible to remove 78% for As(V), 98% for Cd(II), and 99% for Pb(II). Emulsion Liquid Membrane (ELM) is a well-known technique for separating heavy metal ions from wastewater due to the fast extraction and is a single-stage operation of stripping-extraction. The selection of ELM components (Surfactant and Carrier) is a very significant step in its preparation. In the ELM technique, the primary water-in-oil (W/O) emulsion is emulsified to produce water-in-oil-in-water (W/O/W) emulsion. The water in the oil emulsion was prepared by mixing the membrane and internal phases. The extractant D2EHPA (di-2-ethylhexylphosphoric acid) was used as a mobile carrier, Span-80 as a surfactant, and Paraffin as a diluent. Moreover, the internal (receiving) phase was prepared by dissolving sulphuric acid in water. Di-(2-ethylhexyl) phosphoric acid such as surfactant concentration, carrier concentration, sulphuric acid concentration in the receiving (internal) phase, agitation time (emulsion phase and feed phase), the volume ratio of the membrane phase to the receiving phase, the volume ratio of the external feed phase to the primary water-in-oil emulsion and pH of feed were studied on the percentage extraction of metal ions at 20℃. The results show that it is possible to remove 78% for As(V), 98% for Cd(II), and 99% for Pb(II).

• Journal of the Society of Cosmetic Scientists of Korea
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• v.44 no.2
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• pp.125-131
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• 2018

Ascorbic acid (Vitamin C) has been widely used in skin care formulations. Due to its remarkable effects on anti-oxidation, collagen biosynthesis and whitening, ascorbic acid is considered as an effectible anti-aging active ingredient. But, the instability problems of ascorbic acid in cosmetic formulation such as oxidation, browning and changes in smell is the difficult issue to be overcome for the application of high concentration of ascorbic acid. We tried to stabilize the ascorbic acid in non-aqueous liquid formulation that contains polyol solvent at first. The non-aqueous system was effectible to reduce oxidation. But, ascorbic acid was crystallized in the non-aqueous formulation at the low temperature below $5^{\circ}C$. We tried to develop way to stabilize the ascorbic acid in aqueous solutions to solve the crystallizing problem. In this study, we search the optimal ratio of antioxidant combination, such as zinc sulfate, glutathione and curcuma longa (turmeric) root extract. Formulations were stored at - $16^{\circ}C$, $5^{\circ}C$, $25^{\circ}C$, $40^{\circ}C$, $50^{\circ}C$ and cycle($5-40^{\circ}C$) (in incubator) for a period of eight weeks to investigate their stability. In the stability analysis, the test parameters consisted of color, scent, phase separation and sedimentation. Ascorbic acid stability was checked by HPLC analysis.

• Applied Chemistry for Engineering
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• v.25 no.5
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• pp.503-509
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• 2014

The carbon/porous silica composite membrane was fabricated in a simple manner, which could be successfully for the simultaneous separation and production of chiral epoxides and 1,2-diols, based on their differences in hydrophilic/hydrophobic natures. The chiral Co(III)-$BF_3$ salen catalyst adopted in the membrane reactor system has given the very high enantioselectivity and recyclability in hydrolysis of terminal epoxides such as ECH, 1,2-EB, and SO. The optically pure epoxide and the chiral catalyst were collected in the organic phase after hydrolysis reaction. The hydrophilic water-soluble 1,2-diol product hydrolyzed by chiral salen diffused into the aqueous phase through the SBA-16 or NaY/SBA-16 silica composite layer during the reaction. The water acted simultaneously as a reactant and a solvent in the membrane system. One optical isomer was obtained with high purity and yield, and furthermore the catalysts could be recycled without observable loss in their activity in the continuous flow-type membrane reactor.

• KSBB Journal
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• v.23 no.6
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• pp.557-560
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• 2008

The micelle process was developed for pre-purifying paclitaxel from plant cell cultures of Taxus chinensis, giving a high purity and yield. The approach in this work was to transfer paclitaxel in the crude extract to an aqueous surfactant solution as a micelle, allowing organic solvents to be used for removal of lipids and non-polar impurities. In this work, the effects of various surfactants such as CPC, CTMAC, LTMAC, SDS, AOT, Tween, PEG, and Triton were examined on the yield, purity, and phase separation time in micelle process. Among these surfactants, CTMAC (5%, w/v) gave the best result in terms of paclitaxel yield (${\sim}99%$), purity (${\sim}21%$), and phase separation time (30 min). The use of micelles in the pre-purification process allows for rapid and efficient separation of paclitaxel from interfering compounds and dramatically increases the yield and purity of crude paclitaxel for subsequent purification steps.