• Archives of Pharmacal Research
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• v.17 no.3
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• pp.175-181
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• 1994

The solid-phase extraction (SPF) with subsequent tert-butyldimethylsilyl (TBDMS) derivatization was investigated for the rapid profiling and screening of various carboxylated non-steroidal antiinflammatory drugs (NSAIDs) simultaneously in biological fluid samples. Compared to the conventional SPF in adsorption mode using Chromosorb 102, Chromosorb 107, Carbopak B and Thermosorb, the SPF in partition mode using Chromosorb P as the adsorbent, and ethyl acetate/methylene chloride as the eluting solvents provided hightest overall recovenies of the NSAIDs from aqueous solutions with good precision. The solid-phase extracted NASIDs were silylated with N-methyl-N-(tert-butyldimethylsily)trifuoroacetamide to TBDMS derivatives and directly analyzed by capillary gas chromatography and gs chromatography-mass spectrometry. The usefulness of the present method was examined for the profilling and screening of saliva, serum and urine samples for various NSAIDs simultaneously.

• Archives of Pharmacal Research
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• v.19 no.6
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• pp.566-569
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• 1996

A sensitivity method has been developed for the detection and determination of niflmic acid(NA) in human urine. Samples were extracted with diethylether. Flunixin (FN) was added to the sample prior to extraction as an internal standard. Niflumic acid was converted to its methyl derivative and analyzed by capillary gas chromatography/negative chemical isonization mass spectrometry. Using selected ion monitoring (SIM), the levels of NA down to 5 pg/ml could be detected in 5 ml spiked urine sample. Calibration curve was linear over the range of 0.5 ppm-50 ppm. The recovery of niflumic acid from urine at 40 pg/ml was to be $91.7{\pm}3.8(n=3)$ and the coefficient of variation was 4.1%.

• Applied Biological Chemistry
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• v.27 no.4
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• pp.259-263
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• 1984

Volatile flavor components of raw ginseng were collected from the manufacturing process of ginseng extract. Flavor components were separated by capillary column chromatography using SE-54 stationary phase and individual components were identified by means of GC/MS. Twenty six compounds including monoterpenes, esters, ethers, and sesquiterpenoids were tentatively identified. Major flavor components characteristic to ginseng appeared to he sesqiterpenoids such as ${\alpha}-gurjunene,\;{\beta}-maaliene,\;{\alpha}-guaiene,\;{\beta}-patchoulene$, (-)aromadendrene, and ${\beta}-elemene$.

• Journal of Ginseng Research
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• v.8 no.1
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• pp.22-31
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• 1984

Volatile flavor components of fresh ginseng (Panax ginseng C.A. Meyer.) were studied. Steam distillate of fresh ginseng was extracted with ethyl ether and the extract was separated into four fraction: neutral, phenolic, acidic and basis fractions. The ethyl ether concentrates and neutral fraction were analyzed by a combination of SE-54 fused silica capillary gas chromatography and mass spectrometry. Major flavor components of fresh ginseng were predominantly mono(n +2) and sesquiterpenes(n +3) in over two hundred constituents. Of these, 28 were newly identified in volatile flavor components of fresh ginseng by GC-MS.

• Analytical Science and Technology
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• v.8 no.4
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• pp.821-827
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• 1995

Polychlorodibenzo-p-dioxins(PCDDs) have been prepared by microsacale pyrolysis of trichlorophenates. During the pyrolysis reaction, dechlorinated dibenzo-p-dioxins were also formed by the thermolysis of PCDDs. The dechlorination pathways of PCDDs were suggested in this reaction. The identification of these products was performed using capillary column gas chromatography-mass spectrometry.

• Bulletin of the Korean Chemical Society
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• v.17 no.4
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• pp.334-338
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• 1996

Tetra-chlorodibenzo-p-dioxins (tetra-CDDs) were prepared by microscale pyrolysis of trichlorophenates. During the pyrolysis reaction, tri-, di-, and mono-CDDs were also formed by the thermolysis of tetra-CDDs. The dechlorination pathways of tetra-CDDs were suggested for this reaction. The identification of these products was performed with capillary column gas chromatography-mass spectrometry.

• Journal of Pharmaceutical Investigation
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• v.22 no.3
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• pp.197-204
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• 1992

A gas chromatographic method using nitrogen phosphorous selective detection was developed for simultaneous determination of haloperidol and its metabolite, reduced haloperidol, in human plasma. Combelen was used as internal standard, The method involved extraction and trimethylsilylation followed by the injection of $2-4\;{\mu}l$ of benzene layer, which was used to dissolve the trimethylsilylated derivatives of haloperidol and reduced haloperidol, onto SE-54 column [5% phenyl methyl silica fused capillary column, $16m{\times}0.22\;mm$ $(I.D.){\times}0.33\;{\mu}m$ (coated thickness)]. The temperature of column oven was programmed from $200^{\circ}C\;to\;300^{\circ}C$ at the increase rate of $10^{\circ}C/min and also the temperatures of injector and detector were set at $300^{\circ}C$. Helium was used as carrier gas and its flow rate was maintained at 30 ml/min. The detection was conducted with nitrogen phosphorous selective detector. The retention times for combelen, reduced haloperidol and haloperidol were found to be 9.14, 9.75 and 9.99 min, respectively. The detection limits for haloperidol and reduced haloperidol in human plasma were both 0.2 ng/ml. The coefficients of variation of the intra-assay were generally low (below 9.8%). The mean absolute recoveries of added haloperidol and reduced haloperidol from plasma were 72% and 84%, respectively. No interferences from endogenous substances were found.

• Analytical Science and Technology
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• v.8 no.4
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• pp.895-900
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• 1995

Urinary free and acetylated polyamine profiles have been investigated for their potential usefulness as biochemical markers of cancer in a control of group comprised of healthy volunteers (32 cases) and patients with various types of cancers(48 cases). The nine (5 free and 4 acetylated) endogeneous polyamines were simultaneously determined by a sensitive capillary gas chromatography/nitrogen-phosphorus detector (GC/NPD). The newly modified (simple and convenient) method was developed and the compounds were isolated by adsorption onto silica gel and derivatized by heptafluorobutyric anhydride to enhance their specificity on gas chromatograms. The good quality-control data were obtained through the precision and accuracy test and the recovery range of them was 48.6 ~ 101.2 %. The Korean reference values of urinary polyamines were established and significant differences were found in cancer patients compared with normal subjects. Also, to eliminate subject variations, precursors to product concentration ratios were compared between cancer patients and control group. The ratios of both putrescine to spermidine and total (free plus acetylated) putrescine to total spermidine were significantly greater in cancer patients than in normal subjects.

• YAKHAK HOEJI
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• v.41 no.6
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• pp.698-703
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• 1997

Recently, l-deprenyl (selegiline), a relative new antiparkinson`s drug, has been marketed in Korea. As its metabolites, l-methamphetamine and l-amphetamine, are the enantiomers of illicit drugs,d-methamphetamine and d-amphetamine, a method for analysis of enantiomers of methamphetamine and amphetamine in rat urine was investigated. The optical isomers of methamphetamine and amphetamine were analyzed with the chiral derivatizing reagent (S)-(-)-N-(trifluoroacetyl)-prolyl chloride (l-TFP), which was used to form the diastereomers of methamphetamine and amphetamine. And all diastereomers (l-TFP -l-AM, lTFP-d-AM, l-TFP-l-MA & l-TFP-d-MA) were well resolved by capillary gas chromatography. After administration of 10mg/kg l-deprenyl to rat, l-methamphetamine and l-amphetamine were detected without autoracemization to the d form in all urine samples collected during 24hrs, and the ratios of l-amphetamine/l-methamphetamine were 1.1~3.3. l-Amphetamine was detected in only 3 out of 8 urine samples collected during 24~48hrs where as no l-methamphetamine was detected in all cases.

• Korean Journal of Food Science and Technology
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• v.18 no.2
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• pp.105-109
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• 1986

Volatile components of pinenut were identified. Pinenut was extracted by simultaneous distillation and extraction method after Soxhlet extraction. The odor profile of the extract was very similar to that of pinenut. This extract was then fractionated into four fractions by Preparative TLC. These all fractions were analyzed by a combination of glass capillary gas chromatography (FTD, FID capillary GC) and mass spectrometry. One hundred and nine components, including 26 hydrocarbons,17 esters,16 aldehydes,12 ketones,31 alcohols, 11 bases, 2 acids and 3 miscellaneous components were identified.