• Korean Journal of Pharmacognosy
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• v.49 no.3
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• pp.270-277
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• 2018

Pyungwi-san has been used to treat the digestive system diseases, physconia, nausea, anorexia, and dyspepsia in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was optimized for simultaneous determination of the 14 marker components, spinosin, liquiritirn apioside, liquiritin, narirutin, 6'''-feruloylspinosin, hesperidin, liquiritigenin, glycyrrhizin, 6-gingerol, atractylenolide III, honokiol, atractylenolide II, magnolol, and atractylenolide I in Pyungwi-san extract. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) with maintained at $45^{\circ}C$. The mobile phase consisted of 0.1% (v/v) aqueous formic acid and acetonitrile. The MS conditions were as follows: capillary voltage 3.3 kV, extractor voltage 3.0 V, RF lens voltage 0.3 V, source temperature $120^{\circ}C$, desolvation temperature $300^{\circ}C$, desolvation gas 600 L/h, cone gas 50 L/h and collision gas 0.14 mL/min. The coefficient of determination of 14 analytes was 0.9989-1.0000. The limits of detection and quantification values of the all analytes were 0.04-2.56 and 0.13-7.69 ng/mL, respectively. As a result of the analysis using the established LC-ESI-MS/MS method, the 5 components, spinosin, 6'''-feruloylspinosin, atractylenolide III, II, and I derived from Zizyphi Fructus and Atractylodis Rhizoma, were not detected in this extract. On the other hand, the 9 components except for the 5 components were 4.15-498.87 mg/kg in lyophilized Pyungwi-san extract. Among these components, glycyrrhizin, marker compound of Glycyrrhizae Radix et Rhizoma, was detected the most amount as a 498.87 mg/kg.

• Journal of Life Science
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• v.11 no.6
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• pp.568-573
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• 2001

Sea lettuce(Monostrima nitidum) were treated with several alkali agents on condition with water blanching at 9$0^{\circ}C$ for 10 min., and followed by drying and powdering, thus, the power samples treated and the not treated were then allowed to be stored at $25^{\circ}C$, dark place for 5 months. The sea lettuce powder samples were evaluated for green color intensity and volatile flavor at a month intervals. The green intensity of the samples were measured by using Hunter-lab colorimeter, therefore, the decoloration of greenness were seen in both of the samples treated and the not treated, but there were slight inhibitory effects on decoloration in the treated with alkali agents, especially in the treated with KHCO$_3$.The volatile flavor of the samples were collected by simultaneous distillation-extraction, and then the 31 flavor compounds were separated on HP-5 capillary column(25m$\times$0.25mm i.d) and identified by using GC-MS. From these results, it was presumed that the characteristic impact flavor compounds were $\beta$-cyclocitral, $\beta$-cyclohomocitral, ionene, $\alpha$-ionone and $\beta$-ionone. The total content of the characteristic impact flavor compounds decreased in the samples treated with alkali agents more alkali agents more than in the not treated, but lee decrease was observed in the treated with KHCO$_3$.

• Korean Journal of Veterinary Research
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• v.40 no.1
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• pp.63-71
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• 2000

An immunogenic, high molecular weight lipopolysaccharide (LPS)-protein complex isolated from a potassium thioncyanate extract of a Pasteurella multocida (P multocida ; strain P-2383, capsular type A and somatic type 3) was characterized. Chemical analysis of the complex by gas chromatography on a capillary column demonstrated that this complex contained most of the chemical constituents characteristic of LPS extracted by the phenol-water methed from the whole bacterium. However, there was proportionately more carbohydrate than fatty acid in the complex in contrast to LPS in which fatty acid seemed to be in excess. When toxicity of the complex was evaluated in 10-day-old chicken embryos, the complex was less toxic ($LD_{50}=12.72{\mu}g$) than the purified LPS ($LD_{50}=0.44{\mu}g$). The $LD_{50}$, of the LPS moiety extracted from the complex was $5.24{\mu}g$. Composition of the complex was analyzed by SDS-PAGE with silver staining and Western immunoblotting. The complex did not migrate through the polyacrylamide gel unless dissociated with SDS. The complex dissociated with SDS contained at least 32 different protein and polysaccharide components: 18 components reacted with an antiserum against the complex. There was no significant compositional variation between the complexes from different strains, but quantitative differences in individual components were noted. When cross-protectivity of the complex was evaluated in mice, this complex provided substantial protection not only against the homologous bacteriun but also against different P multocida strains of the same serotype. LPS-protein complexes isolated by the same method from other strains also induced protection against an challenge with P-2383.

• Applied Biological Chemistry
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• v.35 no.1
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• pp.36-41
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• 1992

Several commercial cottonseed, corn and rapeseed oils were stored at $60^{\circ}C\;and\;70^{\circ}C$ with daily exposure of fluorescent light for 12 hours and evaluated their rancidity by headspace gas chromatographic analysis of pentanal and hexanal. The data of gas chromatographic analysis was compared with organoleptic flavor evaluation. For headspace gas chromatographic analysis, the volatile compounds were recovered by porous polymer trap and flushed into a fused silica capillary column at $250^{\circ}C$. Twenty-three GC peaks were identified on the basis of relative retention time of reference compounds and gas chromatography-mass spectrometry. The results showed that the contents of pentanal and hexanal were linearly increased during storage. A very simple linear relationship was found between organoleptic flavor scores and amounts of two volatile compounds with very high correlation coefficient. This results suggested the possible implication of pentanal and hexanal as an quality index for rancidity evaluation of cottonseed, corn and rapeseed oils.

• Applied Biological Chemistry
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• v.47 no.4
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• pp.426-429
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• 2004

An easy, sensitive and rapid method for the analysis of phytol, a strong ACAT (Acyl-CoA: Cholesterol Acyltransferase) inhibitory diterpenoid, was established. The pre-treatment of sample for GC analysis of phytol includes aq. MeOH extraction, partition of the extracts between EtOAc and water, and filtration of organic phase through Supelclean LC-Si SPE tube. The GC analysis of phytol for a variety of Lactuca sativa was carried out on DB-5 capillary column with flame ionization detector (FID). The consistency in phytol contents according to each variety was not shown. Especially, Jeoktoma, as RS-2 type, showed the highest phytol content.

• Korean Journal of Food Science and Technology
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• v.22 no.1
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• pp.7-12
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• 1990

The effect of $Fe^{2+}$ and myoglobin on the oxidative stability of triglyceride molecular species was investigated at $25^{\circ}C$. The molecular species of soybean oil triglycerides were analyzed by capillary column gas chromatography and electron impact ionization mass spectrometry utilizing selected ion monitoring. When $Fe^{2+}$ and myoglobin were added to soybean oil triglycerides, the oxidative stability of each molecular species of triglycerides appeared to decrease in proportion to the increase in the number of double bonds present in the acyl residues, and it was affected by degree of unsaturation of fatty acid when the total degree of unsaturation of triglyceride was the same. But the length of the saturated acyl chain had no influence on the stabilization of unsaturated fatty acid present in the same glyceride when prooxidants were added.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.195-203
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• 2015

Quintozene, pentachloronitrobenzene (PCNB) is a contact fungicide for control of soilborne phytopathogenic fungi during cultivation of diverse crops. It was introduced to agricultural use around 1930's as a substitute for mercurial disinfectants. Although quintozene had been first registered in Korea on 1969. However, now it was banned to use due to its high residue levels in selected harvest products. Also, high possibility is expected that the residue may be contained in imported agricultural commodities as it is still used widely over the world. Therefore, this study was conducted to establish a determination method for quintozene residue in crops using GC/ECD/MS. Quintozene residue was extracted with acetonitrile from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and n-hexane partition was followed to recover quintozene from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The quintozene was quantitated by GLC with ECD, using a DB-1 capillary column. The crops were fortified with quintozene at 3 levels per crop. Mean recoveries ranged from 79.9% to 102.7% in five representative agricultural commodities. The coefficients of variation were less than 4.3%. Quantitative limit of quintozene was 0.004 mg/kg in representative five crop samples. A GC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of quintozene in agricultural commodities.

• Korean Journal of Food Science and Technology
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• v.26 no.6
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• pp.665-669
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• 1994

A rapid gas chromatographic (GC) profiling method was applied to dairy products (milk and cheeses) for the simultaneous analysis of volatile and nonvolatile organic acids. Cheese samples were first made into aqueous samples by dissolving in water. The aqueous samples were then extracted with organic solvents after the acidification and NaCI saturation. The organic layers (diethyl ether : hexane= 1 : 1) were extracted with $NaHCO_3$ saturated solution with subsequent solid-phase extraction of the aqueous phases using Chromosorb P column/diethyl ether followed by triethylamine treatment. The resulting triethylammonium salts of acids were directly converted into volatile tert.-butyldimethylsilyl derivatives, which were analyzed by dual-capillary column GC, and GC-mass spectrometry. From milk and four cheese samples studied, 31 organic acids including 21 fatty acids and other hydroxy and dioic acids were tentatively identified. The amounts of the fatty acids were different among the kinds of cheese and thus the simplified retention index (RI) spectra of organic acids were useful for the visual pattern recognition of each sample, when the Direct Comparision method between cheese and a blind sample were attempted, it was quickly recognized to be a gouda cheese with the 999 ppt match quality value.

• Journal of the Korean Society of Food Science and Nutrition
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• v.16 no.2
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• pp.136-146
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• 1987

Flavor components were trapped by stimultaneous steam distillation-extraction method for investigating it in the bellflower roots and fractionated into four groups such as a neutral, a basic, a phenolic and an acidic fraction. An acidic fraction methylated with diazomethane solution and three others were analysed by GC and GC-MS equipping a fused silica capillary column, and S-containing compounds in these were detected with a flame photometric detector (FPD). The total of one hundred and three compounds from the bellflower roots were identified: they were 6 aliphatic hydrocarbons, 10 aromatic hydrocarbons, 2 terpene hydrocarbons, 12 alcohols, 8 terpene alcohols, 17 aldehydes, 3 terpene aldehydes, 5 ketones, 5 esters, 3 furans, 2 thiazoles, 2 lactones, 2 sulfides, 9 phenols, l2 carboxylic acids and 5 others. The greater part of the others except carboxylic acids were identified from a neutral fraction of which was assumed to be indispensable for the reproduction of bellflower root odor in a sensory evaluation. As a result of a sensory evaluation, 1-hexanal, trans-2-hexenal, 1-hexanol, cis-3-hexenol, trans-2-hexenol, 1-octen-3-ol and so forth identified in a neutral fraction were considered to be the key compounds of grass-like odor in the bellflower roots.

• Korean Journal of Environmental Agriculture
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• v.34 no.4
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• pp.309-317
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• 2015

BACKGROUND: An analytical method was developed using GC-ECD/MS to precisely determine the residue of fipronil, a phenylpyrazole insecticide used to control a wide range of foliar and soil-borne pests.METHOD AND RESULTS: Fipronil residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and fipronil was partitioned into n-hexane/dichloromethane (20/80, v/v) to remove polar co-extractives in the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fipronil was separated and quantitated by GC-ECD using a DB-17 capillary column. Accuracy of the proposed method was validated by the recovery from crop samples fortified with fipronil at 3 levels per crop in each triplication.CONCLUSION: Mean recoveries ranged from 86.6% to 106.0% in five representative agricultural commodities. The coefficients of variation were less than 10%. Limit of quantitation of fipronil was 0.004 mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fipronil in agricultural commodities.