• KOREAN JOURNAL OF CROP SCIENCE
• /
• v.51 no.spc1
• /
• pp.166-173
• /
• 2006

Soyasaponins are phytochemicals of major interest fur their health benefits. Chemical investigation of a soybean phytochemical concentrate resulted in the isolation and identification of triterpenoid saponins. The MeOH extraction of defatted hypocotyl separated from soybeans was peformed by the automated solvent extractor (ASE). Fractionation was performed on a flash column ($150mm{\times}40mm$ i.d.) packed with a preparative $C_{18}$ reverse phase bulk packing material $(125\AA,\;55-105{\mu}m)$ and monitored at 210 nm, and collected 14 fractions. Consequent Fsat preparative column liquid chromatography (Fast PCLC) was performed for the purification of Fraction-I (Fr-I) collected from the fraction 8 and 9 of flash chromatography. Fsat PCLC was performed on a Luna $C_{18}\;10{\mu}m,\;100{\AA}$, semipreparative reverse phase column ($250cm{\times}50mm$ i.d.) for the purification of isolated unknown compound (Fr-I-2). Chemical structure of acetyl soyasaponin $A_1\;(MW:1436.6,\;C_{67}H_{104}O_{33})$ was identified and determined by a combination of extensive NMR ($^1H-NMR$, 400 MHz; $^{13}C-NMR$, 100 MHz; DEPT), IR, UV, and ESI-MS analysis.

• Korean Journal of Food Science and Technology
• /
• v.50 no.4
• /
• pp.377-382
• /
• 2018

An HPLC method was developed to quantitate a marker, oxyresveratrol (ORT), for the standardization of mulberry branch extracts (MBE) as a functional ingredient. HPLC was performed on a $C_{18}$ column with a gradient elution using 0.05% $H_3PO_4$ and acetonitrile at a flow rate of 0.8 mL/min, and detected at 320 nm. The HPLC method was validated according to Korea Food and Drug Administration (KFDA) guideline of analytical procedures with respect to specificity, linearity, accuracy and precision. Calibration curve of ORT showed high linearity ($R^2=1$), and limits of detection and quantification were 0.3 and $1.0{\mu}g/mL$, respectively. Relative standard deviation values from intra-and inter-day precision were less than 3.52 and 4.70%, respectively. Recovery rate ranged from 97.64% to 103.69%, and ORT content in MBE was approximately 3.78%. These results suggest that the HPLC method developed for the analysis of ORT in MBE is simple, efficient, and could contribute to the quality control of MBE.

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

• Applied Biological Chemistry
• /
• v.46 no.4
• /
• pp.380-384
• /
• 2003

Optimal extraction, separation and capillary rinsing conditions for capillary electrophoresis (CE) were established to discriminate the geographical origin of ligusticum root (Ligusticum wallichii) using 113 samples (domestic sample n = 62, foreign sample n = 51). Ligusticum root was extracted with 30% ethanol and separated on a uncoated fused-silica $(50\;{\mu}m{\times}27\;cm)$ capillary. Conditions for optimal analysis include: temperature, $40^{\circ}C$; voltage, 10 kV; and pressure injection time, domestic and foreign samples were 5 sec and 2 sec, respectively. The optimal separation buffer was 0.1 M phosphate buffer (pH 2.5) containing 15 mM iminodiacetic acid with 40% methanol. Under the optimal conditions established for CE, the ratio of specific peak area (peak LW-1) to other peak area (peak LW-5) was effective in discrimination geographical origin of ligusticum root. The mean accuracy for correct discrimination of geographical origin of domestic and foreign ligusticum roots were 65% and 63%, respectively.

• The Korean Journal of Pesticide Science
• /
• v.18 no.4
• /
• pp.321-329
• /
• 2014

This experiment was conducted to establish an analytical method for residues of amisulbrom, as recently developed an oomycete-specific fungicide showing inhibition of fungal respiration, in crops using HPLC-UVD/MS. Amisulbrom residue was extracted with acetonitrile from representative samples of five raw products which comprised apple, green pepper, kimchi cabbage, potato and hulled rice. The extract was diluted with 50 mL of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice sample, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, amisulbrom was successfully separated from sample co-extractives and sensitively quantitated by ultraviolet absorption at 255 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery test on every crop samples fortified with amisulbrom at 3 concentration levels per crop in each triplication. Mean recoveries ranged from 85.3% to 105.6% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of amisulbrom was 0.04 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue. The proposed method was sensitive, reproducible and easy-to-operate enough to routinely determine the residue of amisulbrom in agricultural commodities.

• Journal of Microbiology and Biotechnology
• /
• v.21 no.8
• /
• pp.808-817
• /
• 2011

Because of its elevated cellulolytic activity, the filamentous fungus Trichoderma harzianum has a considerable potential in biomass hydrolysis applications. Trichoderma harzianum cellobiohydrolase I (ThCBHI), an exoglucanase, is an important enzyme in the process of cellulose degradation. Here, we report an easy single-step ion-exchange chromatographic method for purification of ThCBHI and its initial biophysical and biochemical characterization. The ThCBHI produced by induction with microcrystalline cellulose under submerged fermentation was purified on DEAE-Sephadex A-50 media and its identity was confirmed by mass spectrometry. The ThCBHI biochemical characterization showed that the protein has a molecular mass of 66 kDa and pI of 5.23. As confirmed by smallangle X-ray scattering (SAXS), both full-length ThCBHI and its catalytic core domain (CCD) obtained by digestion with papain are monomeric in solution. Secondary structure analysis of ThCBHI by circular dichroism revealed ${\alpha}$- helices and ${\beta}$-strands contents in the 28% and 38% range, respectively. The intrinsic fluorescence emission maximum of 337 nm was accounted for as different degrees of exposure of ThCBHI tryptophan residues to water. Moreover, ThCBHI displayed maximum activity at pH 5.0 and temperature of $50^{\circ}C$ with specific activities against Avicel and p-nitrophenyl-${\beta}$-D-cellobioside of 1.25 U/mg and 1.53 U/mg, respectively.

• Journal of Ginseng Research
• /
• v.33 no.1
• /
• pp.8-12
• /
• 2009

A simple gradient HPLC method for rapid determination of major ginsenosides ($Rg_1$ and $Rb_1$) and unique ginsenoside (Rf) of Korean ginseng (Panax ginseng C.A. Meyer) was developed. Within 50min, three ginsenosides have been separated and identified on $\mu$-Bondapak $C_{18}$ column ($3.9{\times}300\;mm$, $10{\mu}m$) with gradient elution using water and acetonitrile as a mobile phase. The method was validated in terms of linearity, accuracy, and precision. The correlation coefficients ($r^2$) for calibration curves of ginsenosides were over 0.9997. The developed HPLC method was successfully applied to the analysis of ginseng samples and the recoveries of ginsenosides were in the range of $101.1{\sim}115%$ with RSD<3.2%. The developed method could be used for rapid evaluation of the ginsenosides $Rg_1$, $Rb_1$, and Rf.

• Current Optics and Photonics
• /
• v.4 no.1
• /
• pp.69-80
• /
• 2020

A Rayleigh Lidar used for wind detection works by transmitting laser pulses to the atmosphere and receiving backscattering signals from molecules. Because of the weak backscattering signals, a lidar usually uses a high sensitivity photomultiplier as detector and photon counting technology for signal collection. The capturing of returned extremely weak backscattering signals requires the lidar to work on dark background with a long time accumulation to get high signal-to-noise ratio (SNR). Because of the strong solar background during the day, the SNR of lidar during daytime is much lower than that during nighttime, the altitude and accuracy of detection are also restricted greatly. Therefore this article describes an ultra-narrow bandwidth filter (UNBF) that has been developed on 354.7 nm wavelength of laser. The UNBF is used for suppressing the strong solar background that degrades the performance of Rayleigh wind lidar during daytime. The optical structure of UNBF consists of an interference filter (IF), a low resolution Fabry-Perot interferometer (FPI) and a high resolution FPI. The parameters of each optical component of the UNBF are presented in this article. The transmission curve of the aligned UNBF is measured with a tunable laser. Contrasting the result of with-UNBF and with-IF shows that the solar background received by a Licel transient recorder decreases by 50~100 times and that the SNR with-UNBF was improved by 3 times in the altitude range (35 km to 40 km) compared to with-IF at 10:26 to 10:38 on August 29, 2018. By the SNR comparison at four different times of one day, the ratio-values are larger than 1 over the altitude range (25~50 km) in general, the results illustrate that the SNR with-UNBF is better than that with-IF for Rayleigh Lidar during daytime and they demonstrate the effective improvements of solar background restriction of UNBF.

• Journal of Oral Medicine and Pain
• /
• v.25 no.4
• /
• pp.415-425
• /
• 2000

In order to obtain the basic data concerning the optimal lasing conditions in using Nd:YAG laser as an adjunctive modality of periodontal therapy of root planing without irreversible structural deterioration of cervical cementum, the author selected 36 human teeth having no cervical abrasion and caries (; 12 anteriors, 12 premolars. 12 molars) extracted due to periodontal diseases, and divided them into 4 groups as Group I, II, III and IV (; each group of 3 anteriors, 3 premolars, 3 molars), and prepared a cementum specimen with thickness of $1.0mm{\pm}0.2mm$ sectioned longitudinally at the middle of mesio-distal thickness (; Group I) or horizontally at 1mm-2mm below the cemento-enamel junction (; Group II, III, IV) from each tooth of each group by low speed diamond wheel saw, and treated them with 0.5 M ethylene diamine tetraacetic acid (; EDTA, pH=7.4) for 2 minutes for elimination of remnants during tooth-sectioning. And the author applied the laser energy from a fiberoptic delivered, free running, pulsed Nd:YAG laser (; wavelength 1064nm. pulse duration $120{\mu}sec$, fiber diameter $320{{\mu}m}$) to cementum surfaces in triplicates of one experiment under the following lasing conditions: 1. stationary mode of fiber in contact to cementum surfaces without air-spray (; Group I )/with air-spray (; Group II), 2. unidirectional moving mode of fiber in contact to cementum surfaces under speed of 3mm-4mm/sec without air-spray (; Group III)/with air-spray (; Group IV), 3. energy per pulse (mJ/pulse) [; energy density ($J/cm^{2}$)] in order of 1.0W/10Hz (100J/pulse); $124J/cm^{2}$, 0.5W/10Hz (50mJ/pulse); $62J/cm^{2}$, 0.4W/10Hz (40mJ/pulse); $50J/cm^{2}$, 0.3W/10Hz (30mJ/pulse); $37J/cm^{2}$, 4. exposure time of 1 second. And the author applied the platinum coating on surfaces of cementum specimens, and evaluated the characteristics of ultrastructural change on surfaces of cementum using the scanning electron microscopy. In general the ultrastructural loss of cervical cementum irradiated under the same lasing condition of laser energy density occurred least in specimens of Group IV. And especially, the ultrastructural loss of cervical cementum irradiated under the laser energy density of $37J/cm^{2}$ almost did not occur in specimens of Group IV. Therefore, it is considered that the pulsed Nd:YAG laser should be applied with the lasing conditions of unidirectional moving mode of fiber in contact to cementum surfaces under speed of 3mm-4mm/sec with air-spray and of laser energy density within $37J/cm^{2}$ as an adjunctive modality of periodontal therapy of root planing without irreversible structural deterioration of cervical cementum.

• Journal of the Korean Chemical Society
• /
• v.25 no.4
• /
• pp.275-282
• /
• 1981

A simple semiquantitative procedure was developed for the determination of sub-ppm level of chromium(VI) in aquatic samples by using an analytical micro-column packed with diphenylcarbazide(DPC) gel beads. DPC gel beads were prepared by swelling XAD-2 resin(115∼150 mesh in dry condition) in ethanol for 10min, packing into a glass column(1.5 mm bore, 65nm length) and adsorbing 1ml of ethanol solution of $2{\times}10^{-3}M$ DPC for 20min at room temperature. When 0.5ml of ethanol solution containing chromium(VI) was passed through the DPC gel column for 40min, the original white color of the reagent gel turned to red-violet from the up-stream of the column. As the length of colored band was proportional to the total amount of chromium(VI) in the sample solution passed through the column, the concentration of chromium(VI) could be determined from the calibration line which had been prepared by using the standard solution. Chromium(VI) ion as small as from 0.1 to 0.8 ppm could be determined with ${\pm}5{\sim}{\pm}15{\%}$ relative errors. Since other interfering cations were few, 100-fold excess of Fe(III), 50-fold excess of Cu(II) could be masked with EDTA. This method was successfully applied to the analysis of chromium(VI) in industrial effluents.