• Analytical Science and Technology
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• 제8권4호
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• pp.829-834
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• 1995

Whole column coldtrapping(WCC) on a fused silica capillary (FSCC)combined with GC/MS analysis was evaluated for use in the investigation of volatile organic compounds(VOCs) in indoor air. Research had indicated that a temperature of $-80^{\circ}C$ is optimal for WCC. Samples were analyzed on a $50m{\times}0.2mm$ cross-linked 5% phenylmethylsilicone fused silica column. Liquid nitrogen was used as the coolant for the peak resolution significantly. The analysis can be performed quickly and conveniently. More than 112 of VOCs were determined in the samples from three typical indoor environment including: (1) a room which had just been decorated involving building materials and paints; (2)a kitchen used for Chinese cooking, and (3) a room had tobacco smoke. The method is could be readily applied to rapid sample screening for VOCs contamination surveys or initial investigations with its valid and simple sampling and analytical technique.

• Korean Journal of Food Science and Technology
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• 제21권3호
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• pp.391-398
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• 1989

Triglyceride molecular species In some vegetable oils were analyzed by capillary column gas chromatography and electron impact ionization mass spectrometry utilizing selected ion monitoring. Triglycerides were separated according to their molecular weights and their degrees of unsaturation on $25m{\times}0.25mm$ fused silica open tubular capillary column coated with a phenylmethylsilicone gum stationary phase and in an analysis time less than 13 min. Triglyceride molecular species were identified by analyzing the fragment ions having the same time on the selected ion monitoring profile . The major triglyceride molecular species in each oils were $C_{18:1}.\;C_{18:2}.\;C_{18:2}(OLL:18.3%),\;C_{18:2}.\;C_{18:2}.\;C_{18:2}(LLL;\;14.3%),\;C_{18:0}.\;C_{18:2}.\;C_{18:2}(SLL;\;14.1%),\;C_{16:0}.\;C_{18:2}.\;C_{18:2}(PLL;\;13.2%),\;C_{16:0}.\;C_{18:2}.\;C_{18:1}(PLO;\;11.6%)$ in corn oil, $C_{18:2}.\;C_{18:2}.\;C_{18:2}(LLL;\;18.0%),\;C_{18:1}.\;C_{18:2}.\;C_{18:2}(OLL;\;18.0%),\;C_{16:0}.\;C_{18:2}.\;C_{18:2}(PLL;\;17.1%)$ in safflower oil, $C_{16:0}.\;C_{18:2}.\;C_{18:2}(PLL;\;23.5%),\;C_{16:0}.\;C_{18:2}.\;C_{18:1}(PLO;\;13.8%),\;C_{18:0}.\;C_{18:1}.\;C_{18:1}(SOO;\;13.5%),\;C_{18:1}.\;C_{18:2}.\;C_{18:2}(OLL;\;10.6%)$ in cottonseed oil.

• Applied Biological Chemistry
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• 제32권4호
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• pp.344-349
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• 1989

Eleven lignan compounds in fruits of Schisandra chinensis BAILLON were identified by gas chromatography/mass spectrometry(GC/MS). The GC/MS conditions were as followed: the GC column used was SPB-1 fused silica capillary $(0.25mm\;id{\times}30m,Supelco)$ and the column oven temperature was programmed from $200^{\circ}C$ to $300^{\circ}C$ at the rate of $4^{\circ}C$ per minute; the MS ionization voltage was 70eV (EI mode). The compounds identified were gomisin J $(M^+;\;388)$, deoxyschizandrin$(M^+;\;416)$, gomisin N $(M^+;\;400)$, schizandrin$(M^+;\;432)$, wuweizisu C $(M^+;\;384)$, gomisin A $(M^+;\;416)$, angeloylgomisin H $(M^+;\;500)$, tigloylgomisin H $(M^+;\;500)$, angeloylgomisin Q $(M^+;\;530)$, gomisin B $(M^+;\;514)$ and benzoylgomisin H $(M^+;\;522)$, peaks of which were separated well on the GC chromatogram.

• Preventive Nutrition and Food Science
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• 제3권2호
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• pp.111-118
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• 1998

To develop a simple, rapid and simultaneous analytical method of phenolic compounds using gas chromatography (GC) and gas chromatography/mass spectrophometer (GC/Ms), this experiment was carried out to search the retention times of capillary columns and the characteristics of fragment ions in electron impact mass spectra. Most of trimethylsilyl derivatives and underivatized phenolic compounds were separated very well on three kinds of capillary columns(HP-1), Ultra-2 and HP-35). Quantitiative determination of phenolic compounds was achieved by internal standards (p-hydroxybenzoic acid iopropyl ester, p-hydroxybenzoic acid ethyl ester). Calibration plts were linear in the investigated range, and the limits of detection were about 5 ng at split mode method. When analyzed by three columns, theseparation times were fairly constant on two nonpolar columns, but a few compounds showed slightly different separation order by the itnermediate polar HP-35 column. The important characteristic patterns of TMS derivatives of phenolic compounds on the EI/MS spectrra appeared at the base peak of [M-15]+ ion and presented at high abundance in most TMS derivatives of phenoloc compounds. [M]+, [M-CH3-COO]+, [M-Si(CH3)4]+ and [M-Si(CH3)4 -CH3]+ also observed in mass spectra of these compounds . Although several compounds have the same retention times on GC column, it might be possible to identify these compounds by the different patternsof mass frgement ions. The TMS derivatives, thus , provide additional information for identification of phenolic compounds in biological systems.

• Archives of Pharmacal Research
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• 제5권2호
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• pp.71-77
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• 1982

Improvements in the analytical methodology used in the gas chromatographic/mass spectral analysis of phenolic compounds from cigarette smoke are described. For the direct analysis of crude samples, pyridine extraction and the glass capillary column GC was used for the separation of phenolics as trimethylsilyl derivativatives. The separations of cigarette smoke on Carbowax 20M and SE-54 wall coated open tubular columns are given. Improved methodology for the routine quantitation of the identified components using the computer-controlled multiple ion selection technique of MS presented. Considerations pertaining to routine analyses of a multitude of complex smoke samples are also discussed.

• Journal of Life Science
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• 제16권2호
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• pp.323-327
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• 2006

The Formation of acrylamide was studied in Maillard model reaction systems based on asparagine-glucose. The mixture of asparagine and glucose in equal molar ratio, and then heated at 125, 150, 175 and $200^{\circ}C$ for 10, 20 and 30 minute, respectively. The reaction products were extracted with ethyl acetate and methanol, and then isolated and detected on FFAP capillary column and HP-5MS 5% phenyl methyl siloxane column by using GC/MS. Acrylamide was detected only from methanol extracts and on FFAP capillary column, at retention time 23.53 min., and the detection limit was 4.6 ng. Acrylamide content mainly increased with increasing temperature and processing time till $175^{\circ}C$, therefore, maximal acrylamide formation occurred at $175^{\circ}C$ for 10 minute ($116{\mu}g/g$), while, above $175^{\circ}C$, higher temperatures or prolonged processing times caused a decrease of acrylamide levels, finally disappeared at $200^{\circ}C$ for 30 minute. Three major compounds were identified as 1,3-dihydroxypropanone, 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyrane-4-one and 5-hydroxymethylfurfural, and three minor compounds also as 5-methylfurfural, 2-acetylpyrrole and N,N-dimethylcyclohexamine, from ethyl acetate or methanol extracts on FFAP or HP-5MS capillary column.

• Applied Biological Chemistry
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• 제32권4호
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• pp.350-356
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• 1989

The determinabilities of several lignan compounds by capillary-GC (F1D) were studied. The lignan compounds used were deoxyschizandrin, gomisin N, schizandrin, wuweizisu C, gomisin A, angeloylgomisin H and tigloylgomisin H which were isolated from fruits of Schisandra chinensis BAILLON and identified with GC/MS(EI, 70eV), 1H-NMR(300MHz) and IR. The GC column used was SPB-1 fused silica capillary$(0.25mm\;ID{\times}30m,\;Supelco)$, and the column oven temperature was programmed from $200^{\circ}C$ to $300^{\circ}C$ at the rate of $4^{\circ}C$ per minute. The linearities between concentration and FID response were maintained in $2{\sim}500ppm$ of deoxyschizandrin and wuweizisu C and in $5{\sim}500ppm$ of gomisin N, schizandrin, gomisin A, angeloylgomisin H and tigloylgomisin H. The contents of lignan compounds in fruits of S. chinensis BAILLON produced at Moo-ju area were analyzed by the GC method: the values obtained of schizandrin and gomisin N were 6.5 and 5.9mg/g respectively, and those of gomisin A, wuweizisu C, angeloylgomisin H, deoxyschizandrin and tigloylgomisin H were $0.5{\sim}1.6mg/g$.

• YAKHAK HOEJI
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• 제26권2호
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• pp.129-132
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• 1982

A GC/MS method was developed to analyze phenolic acid extract from tobacco leaf. Extracted acids were converted to their methyl esters by refluxing with 3M hydrogen chloride in methanol, and the esters were reacted with his (trimethylsilyl) trifluoroacetamide plus 10% trimethylchlorosilane to silylate the phenolic groups. Derivatives of standard salicylic, p-hydroxybenzoic, vanillic, gentisic, p-coumaric, syringic, ferulic, and sinapic acids prepared by this procedure were analyzed by GC/MS on $20m{\times}0.2mm$ column of SE-54 glass capillary. GC/MS analysis of the extract from tobacco leaf revealed the presence of salicylic, p-hydtoxybenzoic, vanillic, gentisic, protocatechuic, p-coumaric, syringic, gallic, ferulic, caffeic, sinapic, and quinic acids, respectively. The quantitative analysis of these phenolic acids were achieved by using multiple ion selection technique.

• Journal of the Korean Chemical Society
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• 제39권8호
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• pp.635-642
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• 1995

Improved sample introduction system has been investigated for the determination of volatile organic compounds in water using a purge & trap preconcentration apparatus and a capillary gas chromatography/mass spectrometry. The present limitations associated with the moisture control module and cryorefocusing system suggested by EPA were discussed. To solve the problems such as improper separation of peaks due to the adsorption of water and contamination of purge & trap system, a more efficient connection system between the purge & trap apparatus and the gas chromatograph was introduced and the optimum operational conditions were suggested. A carbopack B/carboxen 1000 and 1001 trap was used for the purge & trap procedure and a custom made crosslinked dimethyldiphenylpolysiloxane capillary column was used for the separation of compounds. Accuracy and precision of the method suggested in this report were examined and the method detection limit of each compound was proposed for the simultaneous determination of 54 volatile organic compounds in water.

• Journal of the Korean Society of Tobacco Science
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• 제16권2호
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• pp.172-180
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• 1994

This study was carried out to separate and identify the acidic compounds in tobacco leaves. Izmir tobacco leaves was extracted with isopropyl ether and the extract was concentrated. The concentrate was extracted with 6% NaHCO3 aqueous solution. The aqueous extract was acidified with sulfuric acid, and extracted with diethyl ether. The acidic material was fractionated on silicic acid column using a benzene-methanol mixture with a stepwise increasing methanol concentration. The resulting fractions were esterified with diazomethane, and then identified by GC, GC/MS using SPB -5 fused silica capillary column. Most of acidic compounds in Izmir tobacco leaves were elected from fraction B which was benzene-methanol(98 : 2) mixture on silicic acid column chromatography. The identified acidic compounds of Izmir tobacco leaves were 18 saturated acids, 8 unsaturated acids, 5 dicarboxylic acids, 13 aromatic acids and 7 terpenoid acids. The major acidic compounds of lzmir tobacco leaves were 2- methylbutanoic, 3-methyl butanoic, 3- methylpentanoic, hexanoic, nonanedioic, phenylacetic, benzoic, 4- methoxybenzoic, 3, 5- dimethoxybenzoic, methoxycinnamic and 3, 4- dimethoxycinnamic acid. Key Words : Izmir tobacco, Acidic compounds, GC/MS.