• Journal of Life Science
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• v.30 no.11
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• pp.956-964
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• 2020

The radical scavenging activity measurement system linked with liquid chromatography (LC) is a useful tool for identifying the radical scavenging active compound in a sample composed of numerous compounds such as plant extracts. Using this system, DPPH and ABTS radical scavenging activity were measured on extracts of Ulmus pumila cortex, which is known as an herbal medicine with antioxidant activity. Mass spectrometry (MS) was performed on the identified radical scavenging active compounds to identify the four components estimated to be procyanidin B2, procyanidin B3, catechin-7-O-β-D-apiofuranoside, and catechin-5-O-β-D-apiofuranoside, respectively. In order to compare the relative contents between extract samples, multiple reaction monitoring (MRM) mode analysis conditions were set for the four compounds in order to examine the possibility of comparing the content of radical scavenging active compounds in Ulmus pumila cortex extract using LC-MS/MS. As a result of the relative content comparison, it was found that the higher the ethanol concentration of the extraction solvent, the higher the content of radical scavenging active compounds. As with the results of measuring the radical scavenging activity of each extract, it was confirmed that the content difference of three of the compounds (all except the compound estimated as procyanidin B3) was not significantly observed in the extracts with an ethanol concentration of 50% or more.

• The Korean Journal of Food And Nutrition
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• v.16 no.4
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• pp.296-302
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• 2003

First. the purification and analysis of alliin in garlic from different origins by alliin-HPLC determination method were studied. Allinase in garlic was inactivated by heating in boiling water followed by extraction of alliin in garlic with 80% methanol. To remove free amino acids and alliin homologs in garlic, garlic extract was separated by cation exchange column which was packed with amberlite CG-120 resin using 40L d-water as eluent. Alliin in garlic extract was crystallized in a mixture of acetone (50$^{\circ}C$)：H$_2$O：acetic acid=70:29:1 and then recrystallized in a mixture of acetone (50$^{\circ}C$)：H$_2$O：acetic acid=75:24:1. Obtained alliin was identified by melting point. TLC, microscope observation and mass spectrometry. High performance liquid chromatography (HPLC) following pre-column derivatization of cystein derivatives with o-phthaldialdehyde/2-mercaptoethanol has succeessfully been applied to the analysis of various garlics. Each alliic of standard solution and garlic extract was derivatized to isoindole derivative by o-phthaldialdehyde /2-mercaptoethanol and then analyzed by HPLC. Six point calibration was done by using alliin peak area. Lineality was observed at 0 ∼ 1.0mg/ml of alliin concentration. Weighted regression line function was Y=6254X - 256077. By this function, alliin contents in various garlics were 0.34 ∼ 0.73% fresh weight. Second study was designed to evaluate the effects of garlic extracts of various concentrations on the growth of various pathogenes (Eubacterium limonsum, Bacteroides fragilis, Salmonella typhimurium, Salmonella typhi, Shigella sonnei, Kiebsiella pneumoniae, Enterobacter cloacae, Pserdomonas aeruginosa, Escherichia coli). For antimicrobial effects against microorganism, totally minimal inhibition concentrations (MIC) of alliin were from 5,000 to 20,000ppm. MIC of ethanol extract were 1,250 to 10,000ppm.

• Journal of the Korean Society of Food Science and Nutrition
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• v.29 no.6
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• pp.1050-1056
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• 2000

To identify the irradiation-induced volatile flavor compounds, which were not detected in unirradiated sample and had positive correlation with the increment of irradiation dose, the volatile flavor compounds of irradiated (0, 1, 3, 5, 10 kGy) chicken were analyzed by liquid liquid continuous extraction (LLCE) and gas ehromatographyimass spectrometry (GC/MS) methods. One hundred twenty nine compounds were detected in irradiated chicken, and these compounds were composed mainly of hydrocarbons (62 compounds), aromatic compounds (44), aldehydes (9), ketones (5) and miscellaneous compounds (10). Among these, only 3 volatile compounds including 2-methylpentanal (r=0.24), 4-methylcyclohexene (r=0.08) and cyclotetradecene (r=0.92), were detected as irradiation-induced volatile flavor compounds in irradiated chicken. However, only cyclotetradecene was selected as a marker compound for detecting irradiation dosages with high correlation coefficient in irradiated chicken.

• Journal of the Korean Society of Food Science and Nutrition
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• v.29 no.6
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• pp.1042-1049
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• 2000

Irradiation-induced volatile flavor compounds in irradiated (1, 3, 5, 10 kGy) beef were analyzed by liquid liquid continuous extraction (LLCE) and gas chromatography/mass spectrometry (GC/MS) methods. One hundred fifty volatile compounds were detected in irradiated beef. These compounds were composed mainly of 71 hydrocarbons, 35 aromatic compounds, 15 aldehydes, 7 ketones, 4 acids, 6 esters and 12 miscellaneous compounds. Among these, only 6 volatile compounds including (E) -2-hexenal, nonene, 2-nonenal, cyclodecene, dodecene and cyclododecene were detected as irradiation-induced volatile flavor compounds, comparing with unirradiated beef meat. However, 4 volatile compounds, such as cyclodecene (r=0.88), (E)-2-hexenal (r=0.85), nonene (r=0.74) and 2-nonenal (r=0.70), having a positive correlation coefficient with the increment of irradiation dose, were considered as marker compounds for detecting irradiation dosages in irradiated beef.

• The Korean Journal of Pesticide Science
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• v.18 no.3
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• pp.141-147
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• 2014

Fenpyroximate is acaricide of pyrazole group. This acaricide have already been permitted for herb cultivation. This experiment was conducted to establish a determination method for fenpyroximate residue in herbal medicines using HPLC-PDA and HPLC-MS/MS. Fenpyroximate residue was extracted with acetone from samples of herbal which Liquorice Root (Glycyrrhiza uralensis) and Safflower Seed (Carthamus tinctorius Linne). The extract was diluted with saturated saline water and dichloromethane liquid-liquid partition (extraction) was followed to recover fenpyroximate from the aqueous phase. Amino propyl ($NH_2$) and florisil column chromatography was additionally employed for final clean up of the extract. The fenpyroximate was quantitated by HPLC-PDA and HPLC-MS/MS. The herbals were fortified with fenpyroximate at 2 or 3 levels per crop. Mean recovery ratio were ranged from 72.0 to 106.4%. The coefficients of variation were ranged from 0.2 to 4.4. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fenpyroximate in herbal medicines.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.43 no.3
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• pp.201-210
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• 2017

Scutellariae baicalensis (S. baicalensis) has been traditionally used for anti-inflammatory effect. This study was designed to compare the antioxidant and whitening effects of S. baicalensis extract and its fermented extract by Leuconostoc mesenteroides (L. mesenteroides). Fermented extract of S. baicalenins was prepared by inoculation of L. mesenteroides after the extraction procedure with 70% ethanol. S. baicalensis extract and its fermented extract was investigated via high-performance liquid chromatography (HPLC). Simultaneous qualitative analysis of two bioactive components; baicalin and baicalein was achieved by comparing their retention times ($t_R$) and UV spectra with those of the standard components. Cell viability test results indicated that both S. baicalensis extract and its fermented extract were non-toxicity. In DPPH radical scavenging ability, $SC_{50}$ values of the fermented extract was $34.43{\mu}g/mL$ as a result of more effective than S. baicalensis extract. In nontoxic concentration rage, fermented extract of S. baicalensis showed strong melanin production inhibitory effect in ${\alpha}$-melanocyte stimulating hormone (MSH)-stimulated B16F10 cell ($IC_{50}=68.17{\mu}g/mL$). These results suggested that fermented extracts of S. baicalensis has considerable potential as a cosmetics ingredient with an antioxidant and anti-wrinkle and whitening effects.

• Journal of the Korean Chemical Society
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• v.30 no.4
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• pp.369-376
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• 1986

Diosgenin in an Indonesian Costus speciosus was determined by capillary gas-liquid chromatography (GLC). The experimental conditions for the hydrolysis, extraction and acetylation of the diosgenin, and the determination by GLC were investigated. 0.20g of dried sample powder was refluxed in the solution of 3N HCI and xylene at 95∼100${\circ}C$ for 4 hours and the xylene layer was separated. The residue evaporated the xylene was refluxed in 20 : 80 acetic anhydride-pyridine for 30 minutes and the diosgenin acetate was extracted with diethyl ether. Dehydrated with anhydrous $Na_2SO_4$ and evaporated the ether, the residue was dissolved in 5.00ml of n-hexane and injected into GLC. Capillary column of SE-30 25m ${\times}$ 0. 33mm was installed in GLC and the column temperature was increased from 180${\circ}$ to 270${\circ}C$ at rate of 10${\circ}C$/min. The flow rate of carrier gas $N_2$ was 2ml/min and FID was used to detect. The analytical result of the diosgenin was 0.281% and relative standard deviation of 5 measures was 1.8%.

• Korean Journal of Food Science and Technology
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• v.37 no.5
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• pp.723-729
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• 2005

Volatile compounds of dropwort (Oenanthe javanica DC), crown daisy (Chrysanthemum coronarium L. var. spatiosum), and sesame (Sesamum indicum L.) were isolated by steam distillation under reduced pressure (DRP) and liquid-liquid continuous extraction (LLE). Aroma extracts of the plants were identified by gas chromatography (GC) and gas chromatography/mass spectrometry (GC/MS) and their antioxidant activities were evaluated in two different assays. The aroma extracts isolated from dropwort, crown daisy, and sesame inhibited the oxidation of hexanal by 25%, 95%, and 99%, respectively, for one month at the $500{\mu}g/mL$ level. They inhibited malonaldehyde formation from cod liver oil by 48%, 54%, and 29%, respectively, at the $500{\mu}g/mL$ level. Their antioxidant activities were comparable to those of the natural antioxidant, ${\alpha}-tocopherol$.

• Korean Journal of Food Science and Technology
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• v.41 no.4
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• pp.355-361
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• 2009

Polycyclic aromatic hydrocarbons (PAHs) are environmental carcinogenic compounds that arise by several means including food processing methods such as smoking and direct drying and cooking. This study examined the concentration of PAHs in sesame oils with various roasting temperatures (190, 220 and $250^{\circ}C$), methods (direct heating vs. indirect hot air heating), and times (5, 10, 15, 20 and 25 min). The PAHs in the sesame oils were analyzed using liquid-liquid extraction and solid-phase clean up (Florisil), followed by HPLC with fluorescence detection. According to the results, mean levels of total PAHs increased when the sesame oils were roasted at increasing temperatures and times. The sesame oil roasted at $250^{\circ}C$ for 25 min had the highest mean value of total PAHs (4.66 ${\mu}g$/kg). The results of this study suggest that the indirect hot air roasting method decreased PAH formation during sesame oil processing.

• Analytical Science and Technology
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• v.24 no.1
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• pp.1-9
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• 2011

We described an estimation of measurement uncertainty in quantitative analysis of 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THC-COOH), the metabolite of ${\Delta}^9$-tetrahydrocannabinol, in hair samples by using the bead-assisted liquid-liquid extraction and gas chromatography-tandem mass spectrometric (GC-NCI-MS/MS) detection. Traceability of measurement was established through the use of reference materials, calibrated volumetric tubes, volume measuring devices, and measuring instruments. The analytical results were compared and the different contributions to the uncertainty were evaluated. Inter-day variation was performed by using statistical analysis of several indicative factors. Measurement uncertainty associated with the analyte in real forensic hair samples were estimated using QC data. The major factor of contribution to combined standard uncertainty was inter-day repeatability, while those associated with preparation of analytical standard and also sample of weight were insignificant considering the degree of contribution. Relative uncertainty of relative extended standard uncertainty divided into the measured concentration of the analyte was 17% in a hair sample. The uncertainty of result evaluation will be invaluable to improve quality of the analysis.