• Korean Journal of Environmental Agriculture
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• v.37 no.2
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• pp.104-116
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• 2018

BACKGROUND: This experiment was conducted to establish a simultaneous analysis method for 7 kinds of herbicides in 3 different classes having similar physicochemical property as diphenyl ether(bifenox and oxyfluorfen), dinitroaniline (ethalfluralin and trifluralin), and chloroacetamide (metolachlor, pretilachlor, and thenylchlor) in crops using GC-ECD/MS. METHODS AND RESULTS: All the 7 pesticide residues were extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and directly partitioned into n-hexane/dichloromethane(80/20, v/v) to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. The analytes were separated and quantitated by GLC with ECD using a DB-1 capillary column. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop samples fortified with bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries of the 7 pesticide residues ranged from 75.7 to 114.8% 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 the analytes were 0.004 (etahlfluralin and trifluralin), 0.008 (metolachlor and pretilachlor), 0.006 (thenylchlor), 0.002 (oxyfluorfen), and 0.02 (bifenox) 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 residues. Therefore, this analytical method was reproducible and sensitive enough to determine the residues of bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin in agricultural commodities.

• Korean Journal of Environmental Agriculture
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• v.13 no.2
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• pp.199-208
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• 1994

Analytical methods for the determination of the derivatives of the herbicide (${\pm}$)-2-(4-chloro-2-methylphenoxy)propionic acid (MCPP) by capillary column gas chromatography with mass spectrometer (GC-MS) and electron-capture detection (GC-ECD) were studied. A successful procedure was introduced for the ester preparation using $H_2SO_4$, as the catalyst and the alcohol 2,2,2-trichloroethanol (TCE) or 2,2,2-trifluoroethanol (TFE). The identificaiton and elucidation of MCPP by GC-MS spectrometry following the esterification with diazomethane, $BF_3$/methanol, $H_2SO_4$/methanol, TCE, TFE, or pentafluorobenzyl bromide (PFB) were carried out. A comparison of the response-sensitivities among those MCPP esters was made with GC-ECD. Although the methylation product of MCPP was confirmed by GC-MS, its low sensitivity to the ECD limited the detection of MCPP. TCE, TFE, and PFB derivatization methods resulted in a high rate of MCPP esterifications and very sensitive ECD molecular responses. Based on efficiency, convenience, worker safety, and least sample contamination, TFE esterificaiton was considered as the superior method for MCPP analysis to the other methods of derivatization. An accurate method is described for quantifying MCPP in soil leachates by GC-ECD at very low concentrations without the requirement of a complicated clean-up process. As a result, MCPP residues at concentrations of less than $0.1{\mu}g$ in 100ml soil leachate were detected.

• Journal of the Korean Chemical Society
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• v.39 no.2
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• pp.94-102
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• 1995

S-Hydroxypropyl(PH) ${\beta}$-cyclodextrin(hydrophilic), dialkyl(DA)-cyclodextrin(hydrophobic), trifluoroacetyl(TA) ${\gamma}$-cyclodextrin(intermediate) stationary phases were used for gas chromatographic separation of racemic alcohols and their derivatives. All the alcohols used for this experiment were derivatived by using trifluoro acetic anhydride, acetic anhydride, or trichloro acetic anhydride. It is apparent that the enantioselectivity of the enantiomeric pairs was very dependent on the type of acylation reagent. The best experimental condition of optical resolution of the alcohols and their derivatives was different on the polarity of the solute molecules. The chiral separation was also studied depending on temperature, polarity of the column, and hydrogen bonding ability and steric effect between the alchols and CD stationary phase. The chiral recognition mechanism is dependent not upon the kinds of the chiral stationay phases but upon the derivatization of the racemic alchols.

• Journal of the Korean Geotechnical Society
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• v.15 no.1
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• pp.175-183
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• 1999

Recently, problems related to vibrations of decomposed granite soils have acquired increasing attention in Korea because those soils cover approximately one third of the country. Both resonant column and cyclic triaxial test were performed to investigate deformation characteristics of unsaturated and cement-mixed decomposed granite soils in Suwon region. The important soil parameters in this respect are the shear moduli, dynamic moduli of elasticity and damping ratios. The dynamic parameters are influenced by variables such as strain amplitude, ratio of loading cycles, and degree of saturations, etc. Test results and data have shown that the optimum degree of saturation to the maximum shear modulus due to a capillary menisci effect was about 17~18 % at low strain amplitude and 10~15 % at intermediate strain amplitude. This paper suggests the range of threshold strain and mean shear modulus of decomposed granite soils in Suwon region. It also proposed the empirical relationship between the dynamic parameters for cement-mixed and non-mixed decomposed granite soils.

• Korean Journal of Food Science and Technology
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• v.22 no.4
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• pp.405-410
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• 1990

The aroma components of duchung tea and persimmon leaf tea were collected simultaneous distillation and extraction method. Those were analyzed and identified by GC-MS using a fused sillica capillary column. Seventy seven components, including 17 alcohols, 3 hydrocarbons, 15 ketones, 16 aldehydes, 8 esters,8 acids, 8 heterocyclic compounds and 2 phenols were confirmed in duchung tea. Seventy one components, including 17 alcohols, 10 hydrocabrons, 11 ketones, 13 aldehydes, 8 esters, 6 acids, 5 heterocyclic compounds and 1 phenol were confirmed in persimmon leaf tea. The most abundant components of duchung tea were aldehydes(23.31%) including 2-pentenal and heterocyclic compounds(16.71%) including $epoxy-{\beta}-ionone$. The most abundant components of persimmon leaf tea were alcohols(25.57%) including linalool and aldehydes(19.45%) including hexanal and hydrocarbons(10.40%) including ${\alpha}-copaene$.

• Microbiology and Biotechnology Letters
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• v.27 no.6
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• pp.491-499
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• 1999

A great variety of the volatile metabolic by-products was formed in yeast cell during alcohol fermentation. The seibel grape (Vitis labrasca) which was grown in the Southern Korea used for wines. The objective of this research was to identify the volatile flavor compounds during alcohol fermentation and aging at 12$^{\circ}C$. saccharomyces cerevisiae and Schizosaccharomyces pombe were inoculated and fermented in seibel grape must. The volatile flavor compounds of logarithmic, stationary and death phases were extracted, concentrated and identified by gas chromatography/mass spectrometer (GC/MS). The volatile flavor compounds were determined by a Hewlett-Packard 5890 II Plus GC which was equipped with Supelcowax 10 fused silica capillary column (60m$\times$0.32mm$\times$0.25${\mu}{\textrm}{m}$ film thickness) wall coated with polyethyleneglycerol. The scan detection method allowed the comparison of the spectrum from the chromatogram of volatile flavor compounds to those in data Wileynbs base library. Among the volatile compounds collected by ether-hexane extraction method, the evolution of 20 main compounds, such as 9 esters (ethyl butyrate, isoamyl acetate, ethyl caproate, n-hexyl acetate, ethl caprylate, ethyl caprate, diethy succinate, ethyl hexadecanoate, 2-pheneethyl acetate), 4 alcohols (3-methyl-1-butanol, 1-hexanol, 1-heptanol, benzoethanol), 4 ketones and acids (2-octanone, caproic acid, caprylic acid, capric acid), 2 furan and phenol (2,6-bis(1,1-dimethyl ethyl)phenol, 2,3-dihydrobenzofuran) were observed during alcohol fermentation and aging. The production of the esters during alcohol fermentation with S. cerevisiae was higher than those of Sch. pombe. The sensory scores of the aged wine samples in aroma, taste and overall acceptability were not significantly different(p<0.05).

• Bulletin of the Korean Chemical Society
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• v.32 no.7
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• pp.2418-2422
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• 2011

The enantiomeric separation of lactic acid for its absolute configuration has become important task for understanding its biological origin and metabolic process involved in the formation of lactic acid. It involves the conversion of enantiomers as diastereomeric O-pentafluoropropionylated (S)-(+)-3-methyl-2-butyl ester and the direct separation by gas chromatography-mass spectrometry on a achiral capillary column. The (R)- and (S)-lactic acids were completely separated with a high resolution of 1.9. The newly developed method showed good linearity (r ${\geq}$ 0.999), precision (% relative standard deviation = 3.4-6.2), and accuracy (% relative error = -7.7-1.4) with the detection limit of 0.011 ${\mu}g/mL$. When the method was applied to determine the absolute configuration of lactic acid in Lactobacillus delbrueckii subsp. lactis 304 (LAB 304), the composition (%) of (R)-lactic acid in the cell pellet and in the culture medium were $89.0{\pm}0.1$ and $78.2{\pm}0.4$, respectively. Thus, it was verified that the present method is useful for the identification and composition test of lactic enantiomers in microorganisms.

• Journal of the Korean Society of Tobacco Science
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• v.14 no.2
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• pp.159-167
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• 1992

It would be clear that the constituents of the leaf surface lipid is ye비 important as an evaluation index of tobacco leaf quality since the quality of tobacco specific aroma with leaf species depends on the contents of the lipid and the strength of the aroma is determined by the amounts of the lipid secreted. For the reason, a rapid and peproducible method to quantify DVT, which is a kind of lipid, has been studied. The biosynthesis procedure of DVT in leaf growing processes, and the volatile or decompositional characters of DVT in leaf drying processes were also discussed. In consequence, it might be possible to get the data available to the cultivation of better tobacco leaf and the manufacture of cigarettes with better aroma and taste. The results obtained from this study are as follows. 1. Chloroform/dichloromethane solvent was better than chloroform alone for DVT extraction. The extraction yields of the leaf surface lipid were about 5% 2. The extractives with dichloromethane were treated by silylation with BSTPa and the quantitative analysis of DVT was carried out using SE -54 fused silica capillary column. It was found that rapid and reproducible data could be obtained from these methods. 3. In flue - cured tobacco species, DVT contents were $30.3\mu\textrm{g}/cm^2$ in the beginning stage of leaf drying processes and $12.1\mu\textrm{g}/cm^2$ corresponded to 30% levels of the beginning stage, in the end stage. 4. DVT contents in Burley mere 2 times as large as those in fluecured tobacco. DVT in the upper stalk position of leaf was 3 times larger than that in the lower stalk position. 5. DVT of tobacco leaves was decomposed by $SO_2$ gas or the sun light. The decomposition rate was largest in the sample used methanol as a extraction solvent.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.22 no.5
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• pp.370-374
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• 1989

Volatile components in natural and basic fraction of the steam distillation extraction method from squid during processing were analysed by GC and GC-MS equipped with a fused silica capillary column. Thirty eight compounds were identified; they were 31 compounds from neutral, 7 compounds from basic fraction. The main components flavor of squid were 3-methylthiophene, 2-methyl-2-hexanthiol, 1-penten-3-ol, 3-penten-2-ol, 3-ethyl-1,4-hexadiene, 1-hydroxy-2-propanone, hexenal and benzaldehyde etc.. Especially, (E, E)-3,-5-octadecanal were detected during the boiled. 2,5-dimethyl pyrazine, 2-ethyl-6-pyra-zine, 2,3,5-trimethyl pyrazine and 2-ethyl-3,5-dimethyl pyrazine basic compounds, which have respectively a burnt and roasted odor, are considered to be important for the characteristic basic fraction of squid.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.19 no.1
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• pp.45-51
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• 1986

Equimolar aqueous solutions of D-glucose and glycine were heated at $50^{\circ}C\;and\;95^{\circ}C$ at pH 6.7. The headspace volatiles and the ether extracts from the reaction mixture were analyzed by gas chromatography and gas chromatography-mass spectrometry using a fused silica capillary column. The major components formed were identified as diacetyl, three furfurals, two pyrroles, one furanone, two pyranones and two amides. In order to elucidate the formation mechanisms of the amides formed front amino-carbonyl reaction, two model systems were adopted. N-butylacetamide were formed as major components from diacetyl-butylamine ana glyoxal-butylamine systems, respectively. The results obtained suggest that such ${\alpha}-dicarbonyls$ as 3-deoxy-D-erythro-2,3-hexodiulose and diacetyl generated in the amino-carbonyl reaction react with amino compounds, amides then being formed by cleavage of the C-C bond in the ${\alpha}-dicarbonyls$.