• Korean Journal of Environmental Agriculture
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• v.26 no.3
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• pp.246-253
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• 2007

This study was performed to enhance the cleanup efficiency of methoxyfenozide and bentazone by pH adjustment in the course of liquid-liquid partition and to develop an optimum analytical conditions using HPLC coupled with DAD for two matrices, brown rice and rice straw. Preparation procedure of brown rice sample was "extraction${\rightarrow}$coagulation${\rightarrow}$liquid-liquid partition$\rightarrow$-florisil C.C", and this procedure was samely applied to two compounds. In rice straw, preparation procedure of methoxyfenozide sample was "extraction$\rightarrow$-alkalization$\rightarrow$liquid-liquid extraction$\rightarrow$coagulation$\rightarrow$florisil C.C", and in the case of bentazone, "extraction$\rightarrow$alkalization$\rightarrow$liquid-liquid partition$\rightarrow$acidification$\rightarrow$liquid-liquid extraction$\rightarrow$florisil C.C". All these purified samples were redissolved in the mobile phases, acetonitile : 20 mM sodium acetate (75:25, v/v) for methoxyfenozide and acetonitrile : 75 mM sodium acetate, pH 6.0 (40:60, v/v) for bentazone. Recoveries of methoxyfenozide analysis in brown rice and rice straw were 83.5-97.4 and 86.4-97.3%, and detection limits were 0.02 and 0.04 mg/kg, respectively. Recoveries of bentazone in brown rice and rice straw were 86.8-101.9 and 88.3-94.5% and detection limits were 0.005 and 0.01 mg/kg, respectively. This methods seem to be usefully applied to the residue analysis of two compounds in the view of producing stable analytical condition and fair reproducibility.

• Food Science and Biotechnology
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• v.17 no.3
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• pp.475-482
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• 2008

Methanol extracts of peanut (Arachis hypogaea L.) pods were chromatographed, which yielded 3 phytochemicals 1-3 including 5,7-dihydroxychromone (1), eriodictyol (2), and 3',4',5,7-tetrahydroxyflavone (3). To confirm the presence of isolated phytochemicals, the pods extracts were performed by high performance liquid chromatography coupled with a photodiode array detector (HPLC-PDA) and a mass spectrometric detector (MSD) with electrospray ionization (ESI). Optimum extraction conditions for phytochemical contents using peanut germplasm were obtained by employing 90% MeOH for 12 hr at room temperature and phytochemicals 1-3 showed significant differences with concentrations of $407.56{\pm}23.35$, $52.92{\pm}5.11$, and $2,024.34{\pm}134.18\;{\mu}g/g$, respectively. Under this optimal conditions, the contents of phytochemicals 1-3 in peanut pods of 3 Korea cultivars including 'Jakwang', 'Daekwang', and 'Palkwang' exhibited phytochemical 3 was the highest range of $1,338.01-5,162.93\;{\mu}g/g$, followed by phytochemical 1 ($590.13-1,382.10\;{\mu}g/g$), and phytochemical 2 ($25.12-186.85\;{\mu}g/g$), respectively. Moreover, 'Jakwang' exhibited the highest contents of phytochemical (1: $1,362.10{\pm}52.49$, 2: $186.85{\pm}17.69$, and 3: $5,162.93{\pm}148.64\;{\mu}g/g$, respectively), whereas the lowest contents was found in the 'Daekwang' (1: $590.13{\pm}22.23$, 2: $25.12{\pm}2.45$, and 3: $1,338.01{\pm}62.17\;{\mu}g/g$, respectively). These results suggest that the methanol extracts of peanut pods may possess health related benefits to humans owing to various known biological activities of phytochemicals 1-3.

• Resources Recycling
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• v.25 no.4
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• pp.60-67
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• 2016

This study was conducted to establish the adsorption-desorption mechanism and the optimum condition of chromatographic operation for separations of heavy rare earth elements (Gd, Tb, Dy) using a p507-containing resin. By employing Langmuir and Freundlich isotherm together with pseudo first and second order kinetics, absorption-desorption reaction mechanism was investigated. Langmuir and Freundlich isotherm was applied under assumption that adsorption reaction occurs in form of monolayer, and because the result was identical to the assumption, now we know adsorption of heavy rare earth elements occurs in form of monolayer. Concerning the pseudo first and second order kinetic, the pseudo second order seemed to be more suitable to represent heavy rare earth element adsorption mechanism. By using the extraction chromatography to separate heavy rare earth elements, ${\alpha}^{Tb}_{Gd}=1.24$, and ${\alpha}^{Dy}_{Tb}=1.03$ were confirmed in eluent HCl 0.25 M which indicates almost perfect separations of three elements. Furthermore, as concentrations of eluent became higher, the resolution value decreased and the elution area got shortened.

• Analytical Science and Technology
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• v.24 no.6
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• pp.421-428
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• 2011

In this study, headspace disk type monolithic material sorptive extraction (HS-MMSE) was developed, validated and applied to the analysis of volatile aroma compounds from vanilla perfume by gas chromatography -mass spectrometry (GC/MS). HS-MMSE uses monolithic material (MonoTrap) based on silica bonded with octadecyl silane (ODS) and activated carbon as a sorbent. Aroma compounds was adsorbed onto the MonoTrap in headspace and extracted by only 100 ${\mu}L$ of solvent. Total 12 volatile compounds from vanilla perfume were successfully analyzed using HS-MMSE. The influence of extractive parameters was investigated and optimized, using benzyl acetate, linalyl acetate, vanillin, ethyl vanillin as target compounds. Under the optimum condition, the limit of detection (S/N = 3) and the limit of quantification (S/N = 10) of proposed method for the target compounds were obtained within the range of 8.35~13.76 ng and 27.82~45.88 ng, respectively. The method showed good linearity with correlation coefficient more than 0.9888, satisfactory recovery and reproducibility. These results showed that HS-MMSE using disk type MonoTrap is a new promising technique for the analysis of volatile aroma compounds from vanilla perfume.

• Analytical Science and Technology
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• v.18 no.3
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• pp.201-205
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• 2005

Tri-octyl amine (TOA) is used in solvent extraction process for radioactive waste. This compound may be degraded to di-octyl amine (DOA), mono-octyl amine (MOA) by radioactive materials. Amount of TOA, DOA and MOA in TOA must be monitored because they production of these compounds means degradation of which leads to a decrease in the extraction yield. Retention behavior for TOA, DOA and MOA are studied with Phenomenex LUNA-$C_{18}$ ($4.6mm{\times}25cm$) analytical column and $CH_3OH:H_2O$ (50 mmol $CH_3COONH_4$) eluent by liquid chromatography. Optimum condition for these compounds is $CH_3OH:H_2O$ (50 mmol $CH_3COONH_4$) = 85 : 15 ratio. TOA, DOA and MOA compounds is well separated within 20 minute. Dynamic range is $30{\sim}160{\mu}g/mL$ for TOA, $5{\sim}100{\mu}g/mL$ for DOA and $0.1{\sim}5{\mu}g/mL$ for MOA, respectively. The detection limit are $0.1{\mu}g/mL$ for TOA, $1{\mu}g/mL$ for DOA (in SCAN mode) and $0.1{\mu}g/mL$ for MOA (in SIM mode) in this system with $20{\mu}L$ sample loop.

• Journal of the Korean Chemical Society
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• v.37 no.12
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• pp.1035-1046
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• 1993

Some iron(III)porphyrin complexes were prepared, and identified by the spectroscopic methods. Elution behavior of iron(III)porphyrin complexes was investigated by reversed-phase HPLC. The optimum conditions for the separation of iron(III)porphyrin complexes were examined with respect to flow rate and mobile phase strength. These complexes were successfully separated on NOVA-PAK $C_{18}$ column using methanol / water(95/5) for $[T_pCF_3PP)Fe(R)]$ and methanol / water (98/2) for $[(P)Fe(C_6F_5)]$ as a mobile phase. It was found that these complexes were largely eluted in an acceptable range of capacity factor value ($0{\leq}logk'{\leq}1$). The dependence of the capacity factor (k') on the volume fraction of water in the binary mobile phase as well as the dependence of k' on the liquid-liquid extraction distribution ratio$(D_c)$ in methanol-water / n-pentadecane extraction system showed a good linearity. It means that the retention of iron(III)porphyrin complexes on NOVA-PAK $C_{18}$ column is largely due to the solvophobic effect. Also, there was a good linear dependence of the capacity factor(k') on the column temperature and enthalpy calculated by van't Hoff plot. From these results, it was confirmed that the retention mechanism of iron(III)porphyrin complexes in reversed-phase liquid chromatography was invariant under the condition of various temperature, and the solvophobic binding process exhibited isoequilibrium behavior.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.19 no.1
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• pp.20-30
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• 1993

Liquid Chromatographic behavior of Pd(II) in Isonitosoethylacetoacetate imine IEAA-NR: R=H, CH3, C2H5, n-C3H7, n-C4H9, C6H5-CH2) Chelates were investigated by reversed phase high performance 1iquid chromatography on Micropak MCH-5 Column using Methanol /water as mobile phase. The optimum condition for the separation of Pd-Isonitrosoethylacetoacetate imine chelates were examined with respect to the flow rate, mobile phase strength. It was found that Pd(IEAA-NR)2 chelates were eluted in an acceptable range of the capacity factor value (0 $\leq$ log k' $\leq$ 1), The dependence of the logarithm of capacity factor(k') on the volume fraction of water in mixture with in the binary mobile phase was examined. Also, the dependence of k'on the liquid-liquid extraction distribution constant in methanol-water / n-alkane extraction system was on system was invert tigated for Pd(IEAA-NR)2. Both kinds of dependence are linear, which suggests that the retention of the electroneutral metal chelates be largely due to the solvophobic effect.

• Korean Chemical Engineering Research
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• v.56 no.2
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• pp.229-239
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• 2018

The purpose of this study was to effectively produce the biosugar from cell wall of lipid extracted microalgae (LEA) by using microwave-assisted pretreatment without enzymatic hydrolysis process. Response surface methodology (RSM) was applied to optimization of microwave-assisted pretreatment conditions for the production of biosugar based on enzyme-free process from LEA. Microwave power (198~702 W), extraction time (39~241 sec), and sulfuric acid (0~1.0 mol) were used as independent variables for central composite design (CCD) in order to predict optimum pretreatment conditions. It was noted that the pretreatment variables that affect the production of glucose (C6) and xylose (C5) significantly have been identified as the microwave power and extraction time. Additionally, the increase in microwave power and time had led to an increase in biosugar production. The superimposed contour plot for maximizing dependent variables showed the maximum C6 (hexose) and C5 (pentose) yields of 92.7 and 74.5% were estimated by the predicted model under pretreatment condition of 700 w, 185.7 sec, and 0.48 mol, and the yields of C6 and C5 were confirmed as 94.2 and 71.8% by experimental validation, respectively. This study showed that microwave-assisted pretreatment under low temperature below $100^{\circ}C$ with short pretreatment time was verified to be an effective enzyme free pretreatment process for the production of biosugar from LEA compared to conventional pretreatment methods.

• Journal of Korean Society of Environmental Engineers
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• v.22 no.3
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• pp.441-451
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• 2000

Sludge produced from water treatment plants contains plenty of aluminum due to addition of coagulants, polyaluminum chloride(PACI) which has been widely used in most of water treatment plants. however. the whole of PACI is imported from other countries. In this research. the effective methods for recycling PACI from sludge of water treatment plants were developed and evaluated. Aluminum chloride hexahydrate($AlCl_3{\cdot}6H_2O$) was obtained by sparging HCl gas aluminum extracted from sludge using hydrochloric acid (HCI). This aluminum chloride hexahydrate was solidified by decomposition at $180^{\circ}C$. and dissolved in water to produce PACI. The optimum extraction rate was obtained at the condition of 10 minutes of reaction time. $105^{\circ}C$ of reaction temperature. 27.65%(W/W) of HCI concentration. The KS experiment proved that manufactured aluminum chloride hexahydrate was 98.7% degree and the recycled PACI coagulants agreed with the KS standard. The optimum temperature of decomposition was $180^{\circ}C$ and the basicity of the PACI was decided upon the extent of decomposition The compared experiments between purchased coagulant and manufactured coagulant presented that both coagulants had same performance for turbidity, DOC, $UV_{254}$ absorbance. and chlorophyll-a.

• Korean Chemical Engineering Research
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• v.54 no.4
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• pp.443-447
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• 2016

The microalgae have cellulose as a main structural component of their cell wall and the lignin content in microalgae is much lower than other lignocellulosic biomass. Therefore, fermentable sugar production from microalgae (Tetraselmis KCTC 12236BP) can be carried out under pretreatment without high temperature and high pressure. It was investigated that the effect of hot-water pretreatment using sulfuric acid for lipid extracted algae which is expected to be a next generation biomass. The effects of three major variables including extraction temperature, acid concentration and time on the enzymatic hydrolysis were investigated. Among the tested variables, temperature and acid concentration showed significant effects and optimum pretreatment conditions for the economic operation criteria were obtained as follows: reaction temperature of $120^{\circ}C$, sulfuric acid concentration of 2 mol and pretreatment time of 40 min. Under the optimum conditions of acidic hot water pretreatment, experimentally obtained hydrolysis yield were 95.9% which showed about 2.1 fold higher compared with enzymatic hydrolysis process. Therefore, acid pretreatment under mild condition was proven to be an effective method for fermentable sugar production from lipid extracted microalgae.