• Analytical Science and Technology
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• v.35 no.6
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• pp.256-266
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• 2022

It is important to determine the concentration of long-lived radionuclides (e.g., ¹²⁹I) in nuclear waste to ensure safety when handling it. To analyze nuclides in a solid sample (e.g., concrete and soil), it is essential to effectively separate and purify the nuclides of interest in the sample. This study reports the comprehensive efforts made to validate the analytical procedure for ¹²⁹I detection in solid samples, using a high-temperature combustion furnace. ¹²⁹I volatilized from the sample collected in 0.01 M HNO₃ solution with a reducing agent (e.g., NaHSO₃) and was rapidly measured by ICP-MS. Analytical conditions, such as pyrolysis temperature and types of mobile phase gas, catalyst, and trapping solution, were optimized to obtain a high recovery rate of spiked ¹²⁹I. Finally, the optimized method was applied for the simultaneous analysis of other volatile radionuclides, such as ³H and ¹⁴C. The performance test results for the optimized method confirmed that the LSC (for ³H and ¹⁴C) and ICP-MS (for ¹²⁹I) measurements, with the separation of volatile nuclides using a high-temperature combustion furnace, were reliable.

• Korean Journal of Food Science and Technology
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• v.44 no.6
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• pp.686-691
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• 2012

The objective of this research is to present method development and validation for the simultaneous determination of lutein and zeaxanthin using ultra performance liquid chromatography (UPLC). Also, rapid quantification was performed on six green leafy vegetables (Allium tuberosum, Aster scaber, Hemerocallis fulva, Pimpinella brachycarpa, Sedum sarmentosum and Spinacia oleracea) that are commonly consumed in Korea. Separation and quantification were successfully achieved with a Waters Acquity BEH C18 ($50{\times}2.1mm$, $1.7{\mu}m$) column by 85% methanol within 5 min. Two compounds showed good linearity ($r^2$ > 0.9968) in $1-150{\mu}g/mL$. Limit of detection (LOD) and quantification (LOQ) for lutein and zeaxanthin were 1.7 and 5.1 g/mL and 2.1 and 6.3 g/mL, respectively. The RSD for intra- and inter-day precision of each compound was less than 10.69%. The recovery of each compound was in the range of 91.75-105.13%. Aster scaber and Spinacia oleracea contained significantly higher amounts of lutein ($4.06{\pm}0.24$ and $3.97{\pm}0.10mg$/100 g of fresh weight), respectively.

• Herbal Formula Science
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• v.21 no.2
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• pp.133-143
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• 2013

Objectives : We carry out the simultaneous quantification for quality control of four components in Bangpungtongseong-san (BPTSS) sample. In addition, we assessed the antioxidant effects of BPTSS sample. Methods : The used column for separation and analysis of four compounds was Luna C18 column and column oven temperature was maintained at $40^{\circ}C$. The mobile phase for simultaneous determination consisted of two solvent systems, 1.0% acetic acid in water and 1.0% acetic acid in acetonitrile. High performance liquid chromatography-photodiode array (HPLC-PDA) method for analysis was performed at a flow rate of 1.0 mL/min with PDA detection at 254 and 280 nm. The injection volume was 10 ${\mu}L$. The antioxidant activities of BPTSS were evaluated by measuring free radical scavenging activities on 2,2'-Azinobis-3-ethyl-benzothiazoline-6-sulfonic acid (ABTS) and 1-1-diphenyl-2-picrylhydrazyl (DPPH). The inhibitory effects on low-density lipoprotein (LDL) oxidation were evaluated by the formation of thiobarbituric acid relative substances (TBARS) and relative electrophoretic mobility (REM). Results : Calibration curves were acquired with $r^2{\geq}0.9999$. The values of limit of detection (LOD) and quantification (LOQ) were 0.06-0.29 ${\mu}g/mL$ and 0.20-0.98 ${\mu}g/mL$, respectively. The amounts of geniposide, liquiritin, baicalin, and glycyrrhizin in BPTSS were 5.06, 7.33, 27.56, and 7.81 mg/g, respectively. The BPTSS showed the radical scavenging activity in a dose-dependent manner. The concentration required for 50% reduction (RC50) against ABTS and DPPH radicals were 72.51 ${\mu}g/mL$ and 128.49 ${\mu}g/mL$. Furthermore, GMGHT reduced the oxidation properties of LDL induced by CuSO4. Conclusions : The established HPLC-PDA method will be helpful to improve quality control of BPTSS. In addition, BPTSS has potentials as therapeutic agent on anti-atherosclerosis.

• Journal of Energy Engineering
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• v.23 no.4
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• pp.141-149
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• 2014

In the present study, pure RHO zeolite was hydrothermally synthesized by using 18-crown-6 ether as a structure directing agent(SDA), and the small gases adsorption was investigated. Synthesized RHO zeolite was a cube shape particle of which average edge length was around $1.2{\mu}m$ and composed of primary crystallites having a diameter of around 100 to 200 nm. RHO zeolite structure was stable under 3h calcination at $600^{\circ}C$. Water adsorption data announced that RHO zeolite has a specific surface area of 483.32 m2/g and its micropore diameter was about 4 A. Gas adsorption was studied in the pressure range of 50 to 500 kPa for $CO_2$, $N_2$, $O_2$ and $H_2$. It was evident that RHO zeolite showed a strong $CO_2$ adsorption behavior. Especially, RHO zeolite showed a transient $CO_2$ adsorption behavior. The 3h $CO_2$ up-take at 50 kPa and 500 kPa was 1.283 and 3.357 mmol/g, respectively. The $CO_2/H_2$ selectivity was around 16 at 500 kPa. Compared with gas adsorption data for some representative microporous adsorbents, it was certain that RHO zeolite is a beneficial adsorbent for $CO_2/H_2$ separation.

• Bulletin of the Korean Chemical Society
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• v.34 no.9
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• pp.2760-2764
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• 2013

Geniposide is a biologically active ingredient of gardenia fruit. A liquid chromatography-tandem mass spectrometric method was developed and validated for the determination of geniposide in rat plasma. The plasma samples were pretreated by solid-phase extraction and introduced into a BDS Hypersil $C_{18}$ column ($50{\times}2.1mm$, $5{\mu}m$) for chromatographic separation. The mobile phase consisted of 0.1% formic acid and 0.1% formic acid in acetonitrile, and gradient elution was performed at a flow rate of 0.25 mL/min. For mass spectrometric detection, multiple reaction monitoring was performed via an electrospray ionization source in positive mode. The calibration curve for geniposide was linear ($r^2=0.997$) in the concentration range of $0.005-1{\mu}g/mL$. The intra- and inter-day accuracies and precisions fulfilled the required criteria (${\pm}15%$). The developed method was subsequently used for pharmacokinetic analysis of geniposide after oral administration to rats at a dose of 50 mg/kg. The mean maximum plasma concentration of geniposide was $0.68{\pm}0.29{\mu}g/mL$ at $0.44{\pm}0.13h$, and the mean area under the plasma concentration versus time curve was $1.46{\mu}g{\cdot}h/mL$.

• Analytical Science and Technology
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• v.32 no.3
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• pp.96-104
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• 2019

Agastache rugosa, known as Korean mint, is a medicinal plant with many beneficial health effects. In this study, a simple and reliable HPLC-UV method was proposed for the quantification of rosmarinic acid (RA) in the aqueous extracts of A. rugosa. RA was selected as a quantification marker due to its easiness in procurement and analysis. The developed method involved chromatographic separation on a $C_{18}$ column ($250{\times}4.6mm$, $5{\mu}m$) at room temperature. The mobile phase consisted of water and acetonitrile both containing 2 % acetic acid and was run at a flow rate of $1mL\;min^{-1}$. The method was validated for specificity, linearity, precision, and accuracy. It was specific to RA and linear in the range of $50-300{\mu}g\;mL^{-1}$ ($r^2=0.9994$). Intra-day, inter-day, and inter-analyst precisions were ${\leq}0.91%\;RSD$, ${\leq}1.40%\;RSD$, and 1.94 % RSD, respectively. Accuracy was 93.3-95.9 % (${\leq}1.21%\;RSD$). The method could be applied to three batches of bulk samples and three batches of lab scale samples, which were found to be $0.64({\pm}0.04)mg\;g^{-1}$ and $0.48({\pm}0.02)mg\;g^{-1}$ for the dried raw materials of A. rugosa. The results show that the proposed method can be used as a readily applicable method for QC of health functional foods containing the aqueous extracts of A. rugosa.

• Bulletin of the Korean Chemical Society
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• v.32 no.8
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• pp.2637-2642
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• 2011

A new ultrasonic-assisted micellar extraction and cloud-point pre-concentration method was developed for the determination of major saikosaponins, namely saikosaponins -A, -C and -D, in Radix Bupleuri by high performance liquid chromatography with evaporative light scattering detection (HPLC-ELSD). The non-ionic surfactant Genapol X-080 (oligoethylene glycol monoalkyl ether) was chosen as the extraction additive and parameters affecting the extraction efficiency were optimized. The highest yield was obtained with 10% (w/v) Genapol X-080, a liquid/solid ratio of 200:1 (mL/g) and ultrasonic-assisted extraction for 40 min. In addition, the optimum cloud-point pre-concentration was reached with 10% sodium sulfate and equilibration at $60^{\circ}C$ for 30 min. Separation was achieved on an Ascentis Express C18 column (100 ${\times}$ 4.6 mm i.d., 2.7 ${\mu}M$) using a binary mobile phase composed of 0.1% acetic acid and acetonitrile. Saikosaponins were detected by ELSD, which was operated at a $50^{\circ}C$ drift tube temperature and 3.0 bar nebulizer gas ($N_2$) pressure. The water-based solvent modified with Genapol X-080 showed better extraction efficiency compared to that of the conventional solvent methanol. Recovery of saikosaponins ranged from 93.1 to 101.9%. An environmentally-friendly extraction method was successfully applied to extract and enrich major saikosaponins in Radix Bupleuri.

• KSBB Journal
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• v.22 no.3
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• pp.174-178
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• 2007

The aim of this study was to identifyisothiocyanates (ITCs) from wasabi (Wasabi japonica Matsum) using supercritical carbon dioxide ($SCO_2$) and to compare the composition in the extracts between $SCO_2$ and organic solvents extraction. A semi-continuous high pressure apparatus was used to extract wasabi (roots, stems and leaves) at following conditions pressure 80$\sim$120 bar, temperature $40\sim50^{\circ}C$. Ether, ethanol, chloroform and dichloromethane were used as organic solvents. The ITCs extracted by means of both separation technologies were analyzed by a gas chromatography system. As the results of study, AITC and ITCs were highly extracted at 40$^{\circ}C$ and 80 bar. To extract AITC from wasabi, $SCO_2$ extraction is more effective than organic solvents extraction, resulted in thermal degeneration and remaining of organic solvents.

• The Korean Journal of Food And Nutrition
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• v.11 no.2
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• pp.179-184
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• 1998

As a way of mass process of onion, Allium cepa L., the oleoresin decompressed and concentrated is an alternative process to minimize lowering in the quality of onion during storage, to improve the original flavor and taste, and to increase variety as processing aids. This study was performed to investigate on the quality stability during storage of oleoresin. Oleoresin product was manufactured by mixing a concentration of onion juice and ethanol extract homogenously, emulsified by an additional 2% PGDR(polyglycerol condensed ricinoleate) and 1% cysteine. During 60 days storage at 5$^{\circ}C$, $25^{\circ}C$ and 4$0^{\circ}C$ the total sugar content in oleoresin product was very stable, and absorbances at 420nm as browning reaction index were 0.38, 1.53 and 3.32, respectively, addition of 1% cysteine retarded the browning reaction effectively. When oleoresin product was centrifuged(2000$\times$G, 60 minutes), the volumes of emulsion level without separation were 96.8%, 94.1% and 9.06%, respectively during 20 days, 40 days and 60 days storage at 5$^{\circ}C$, and those during 60 days storage at $25^{\circ}C$ and 4$0^{\circ}C$ were appeared to be 83.2% and 75.4%. Showing lower level as increasing storage temperature. Antioxidant indexes(AI) of soybean oil added 1% oleoresin without storage and 0.02% BHA were 1.39 and 1.72. The former showed 80.8% antioxidant activity on induction time extension effect of the latter. Antioxidant indexes of oleoresin decreased slightly as increasing storage temperature and were 1.37, 1.30 and 1.08. Total pyruvate contents were 89.9%, 79.7% and 65.2%, respectively during 60 days storage at 5$^{\circ}C$, $25^{\circ}C$ and 4$0^{\circ}C$. Rate constant, Q10 value and activation energy were 1.381~4.735 mmol/$\ell$.hr, 1.537~1.694 and 11.649 ㎉/g mole for the reduction of pyruvates in the range of storage temperatures during oleoresin storage.

• Applied Chemistry for Engineering
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• v.16 no.1
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• pp.123-130
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• 2005

Zeolite X adsorbents with large surface area were prepared for using oxygen PSA adsorbent. Selective adsorption performance of nitrogen on the synthesized zeolite X adsorbent was improved by the cation exchange of adsorbent. The zeolite X which had over $650m^2/g$ surface area was synthesized at the conditions of $SiO_2\;:\;Na_2O\;:\;H_2O\;:\;Al_2O_3$ = 2.5 : 3.5 : 150 : 1 mole ratio, $98^{\circ}C$ temperature and 18 h synthesized time in 50 L reactor. The metal ions Li, Ag, Ca, Br, Sr, etc. were investigated for ion exchange with zeolite X. Ag ion was showed the highest ion exchange rate among these metal ions and all metal ions were exchanged with Na ion at equivalent rate. Compared with the NaX adsorbent, the ion exchanged zeolite X adsorbent remarkably improved its adsorption performance of nitrogen at the conditions of $10{\sim}40^{\circ}C$ temperature and 0~9 atm pressure. At an equilibrium pressure under 0.5 atm, adsorption performance of nitrogen on the ion exchanged zeolite adsorbent increased in the order of Ag > Li > Ca > Sr> Ba > K, whereas at an equilibrium pressure over 1 atm showed in the order of Li > Ag > Ca > Sr > Ba > K. Nitrogen/oxygen separation factor of Li ion exchanged zeolite X adsorbent was 13.023 at the partial pressure of nitrogen/oxygen gas mixture similar to air and $20^{\circ}C$ adsorption temperature.