• Analytical Science and Technology
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• v.8 no.4
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• pp.739-744
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• 1995

The two main methods to prepare water samples for analyzing volatile organic compounds(VOC's) were investigated. One is the purge and trap(PT) method and another is the head space(HS) sampling method. Both methods were effective to transfer the low boiling point components from the water sample onto the capillary column. The cryo-focusing at the top of the main capillary column was an effective way to obtain the sharpness of the chromatographic peaks but could be avoided when a semi-wide bore column was used. The recovery from the same amount of the sample was better in PT than in HS but a larger sample volume in HS method could compensate the lower efficiency. Therefore PT is suitable to the analysis of drinking water where the very low concentration must be determined. HS is suitable to waste water analysis because of the easiness of the operation. The repeatability was good and similar in both methods. For the contamination of the former sample, both methods were tough and could be used without any problems. The matrix effect which could change the equilibrium parameters in HS method was find negligible in many components. The actual samples such as tap water and river water were analyzed with both methods concerning 16 components regulated in Korea.

• Journal of the Korean Society of Food Science and Nutrition
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• v.23 no.2
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• pp.261-267
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• 1994

Parched mugwort tea was manufactured from mugwort (Artemisia asicatica nakai) leaves by traditional green tea preparation method. Volatile flavor compounds were collected by Tenax GC and they separated on DB-5 capillary column ($60m\;\times\;0.25mm$ i.d.) Fifty eight compounds were isolated and identified by GC-MS from the volatiles. Eleven compounds incucluding benzaldehyde, pinene, myrcene, cineole, 2-phrrolidinonoe, camphor, thujong, 1-acetylpiperidine, caryophyllene, coumarin, and farnesol among the compounds identified were considered as important compounds contributing mugwort-like flavor to the parched mugwort tea. The mixture of these eleven authentic compounds could reproduce aroma of mugwort leaves harvested in April. As results, the concentrations of these eleven flavor compounds in parched mugwort tea may indicate the strength of mugwort-like aroma of the tea.

• Korean Journal of Environmental Agriculture
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• v.29 no.2
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• pp.165-175
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• 2010

A gas chromatographic (GC) method was developed to determine residues of captan, folpet, captafol, and chlorothalonil, known as broad-spectrum protective fungicides for the official purpose. All the fungicide residues were extracted with acetone containing 3% phosphoric acid from representative samples of five agricultural products which comprised rice, soybean, apple, pepper, and cabbage. The extract was diluted with saline, and dichloromethane partition was followed to recover the fungicides from the aqueous phase. Florisil column chromatography was additionally employed for final cleanup of the extracts. The analytes were then determined by gas chromatography using a DB-1 capillary column with electron capture detection. Reproducibility in quantitation was largely enhanced by minimization of adsorption or thermal degradation of analytes during GLC analysis. Mean recoveries generated from each crop sample fortified at two levels in triplicate ranged from 89.0~113.7%. Relative standard deviations (RSD) were all less than 10%, irrespective sample types and fortification levels. As no interference was found in any samples, limit of quantitation (LOQ) was estimated to be 0.008 mg/kg for the analytes except showing higher sensitivity of 0.002 mg/kg for chlorothalonil. GC/Mass spectrometric method using selected-ion monitoring technique was also provided to confirm the suspected residues. The proposed method was reproducible and sensitive enough to determine the residues of captan, folpet, captafol, and chlorothalonil in agricultural commodities for routine analysis.

• Analytical Science and Technology
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• v.19 no.4
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• pp.352-364
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• 2006

This study was performed to search for useful separation properties and elution orders of three GC columns (DB-1, DB-5MS, SPB-Octyl) for 209 PCBs congeners using M-1668A-0.01X-SET of the AccuStandard Inc.. In addition, to confirm the quantitative peak in peak pattern method, the IUPAC Nos. of PCBs congener peaks were identified with 4 Aroclor standards (Aroclor-1242, 1248, 1254 and 1260). The separation property of dioxin-like PCBs congeners by four columns (DB-1, DB-5MS, SP-2331 and SPB-Octyl) was excellent in SP-2331. DB-1 and SPB-Octyl columns are necessary to use with a column of other types.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.22 no.4
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• pp.169-176
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• 1989

Volatile flavor components in powdered Katsuobushi were simultaneous trapped by steam distillation-extraction method, and these were fractionated into the neutral, the phenolic, the acidic and the basic fraction. Volatile flavor components in these fraction were analyzed by the high-resolution GC and GC-MS equipped with a fused silica capillary column. The whole steam volatile concentrate consisted of $48\%$ neutral fraction(NF), $35\%$ phenolic fraction(PF), $12\%$ acidic fraction(AF) and $5\%$ basic fraction(BF). Thirty components such as 8 hydrocarbons, 8 aldehydes, 6 furans, 5 alcohols and 3 ketones were identified from NF. And sixteen components such as phenol, guaiacol, dimethoxy phenol, eugenol in PF, twelve components such as propionic, butanoic, isopentanoic, n-hexanoic, heptanoic, octanoic acid in AF, ten components such as 2,6-dimethylpyrazine, 2-nethylpyridine, 2,4-dimethylthiaBole in BF were identified. NF and PF gave a much higher yield than others and were assumed to be indispensable for the reproduction of aroma of powdered Katsuobushi. It was also identified eight components of volatile carbonyl compounds such as ethanal, propanal, butanal, pentanal by 2,4-DNPH method.

• Analytical Science and Technology
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• v.24 no.5
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• pp.352-359
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• 2011

An analytical method for solvent-free determination of benzene, toluene, ethylbenzene, and xylenes (BTEX) in water using repetitive membrane extractions coupled to cryofocusing and GC-MS was derived. BTEX compounds that permeated through a nonporous silicone membrane from the aqueous phase and evaporated into the acceptor phase were purged into a cryofocusing trap ($-100^{\circ}C$) with helium gas. The BTEX compounds, thus enriched in the trap, were thermally desorbed into a capillary column GC and detected using an MS. The flow rate of the donor phase (30 mL water) was set at 10 mL/min, and membrane extractions, accomplished by returning the water drained from the extraction module to the sample container, were repeated three times at $20{\pm}2^{\circ}C$. Although recoveries (%) were variable, from the highest for benzene (approximately 80%) to the lowest for ethylbenzene and xylenes (3.5-10%), the method showed satisfactory precision (RSD 2.2-10%) with good-linearity calibration curves ($r^2$ 0.9976-0.9997 in 1-100 ${\mu}g$/L range) for all of the compounds. The method detection limits (MDLs) ranged from 0.16 to 1.8 ${\mu}g$/L. The results showed the method's advantages such as short analysis time and overall simplicity without solvent compared to the conventional techniques.

• Applied Biological Chemistry
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• v.36 no.6
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• pp.424-427
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• 1993

The chloroform extract of mustard leaves (Brassica juncea Cosson) reduced mutagenicity of $AFB_1$ in bacterial assay (Salmonella typhimurium TA100). 4-Decanol was one of major compounds in the chloroform extract when analyzed by GC-MS on HP-5 capillary column. The authentic compound of 4-decanol dissolved in DMSO (0.5%) inhibited mutagenic activities of $AFB_1$ and MNNG in Salmonella typhimurium TA100 at a rate of 99% and 93%, respectively. This result indicates that 4-decanol is an antimutagenic compound present in chloroform extract of mustard leaves.

• The Korean Journal of Pesticide Science
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• v.4 no.1
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• pp.1-10
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• 2000

The purpose of this study is to establish the assessment techniques of hazardous chemicals by the development of analytical method of biological samples. In this study, we have developed an extraction method of nine pesticides used for rice paddy that resulted in high recovery from the spiked human urine by the liquid-liquid extraction with diethyl ether at pH 7.0. Calibration curve obtained from each pesticide standard using by gas chromatography/mass spectrometry/selected ion monitoring has shown good linearity and detection limits were the range of $0.4{\sim}2.0$ ng/mL in urine. As a biological monitoring, urine samples of local farmers exposed directly to nine pesticides in the field were collected and analyzed by GC/MS. Of the tested pesticides, metabolites of phenthoate assumed were identified by GC/MS analysis. No parent compound was detected.

• Korean Journal of Food Science and Technology
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• v.26 no.2
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• pp.162-166
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• 1994

A rapid gas chromatographic (GC) profiling method for the simultaneous analysis of volatile and nonvolatile organic acids was applied to alcoholic beverages (white wine, red wine, brandy, and beer). It involves the solid-phase extraction of organic acids using Chromosorb P as the sorbent and diethyl ether as the eluent with subsequent triethylamine treatment. The resulting triethylammonium salts of acids were directly converted to volatile tert.-butyldimethylsilyl derivatives, which were analyzed by dual-capillary column GC and GC-mass spectrometry. From the alcoholic beverages studied, more than 29 organic acids were detected. When the simplified retention infer (RI) spectra of organic acids, and the direct comparisor method between alcoholic beverages and a test sample were attempted to identify a test sample, it was quickly recognized to be a red wine with the 998 ppt match quality value.

• 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.