• Bulletin of the Korean Chemical Society
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• v.19 no.11
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• pp.1189-1193
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• 1998

The determination of total paraffin, naphthene, and aromatic (PNA) contents in naphtha samples, which were directly obtained from actual refining process, has been studied using near-infrared (NIR) spectroscopy. Each of the total PNA concentrations in naphtha has been successfully analyzed using NIR spectroscopy. Partial least squares (PLS) regression method has been utilized to quantify the total PNA contents in naphtha from the NIR spectral bands. The NIR calibration results showed an excellent correlation with those of conventional gas chromatography (GC). Due to its rapidity and accuracy, NIR spectroscopy is appeared as a new analytical technique which can be substituted for the conventional GC method for the quantitative analysis of petrochemical products including naphtha.

• Proceedings of the PSK Conference
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• 2003.10b
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• pp.68.1-68.1
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• 2003

A method for determination 11 endocrine disrupting chemicals of phenols in various samples was deloped. The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) followed by two work-up methods for comparison; isobutoxycarbonyl (isoBOC) derivatization method and tert-butyldimethylsilyl (TBDMS) derivatization method. Eleven endocrine disrupting chemicals (EDCs) of phenols in biological samples were extracted with acetonitrile and then acetonitrile layer was refrigerated at -60$^{\circ}C$ for 2 hours (freezing filtration). (omitted)

• Journal of Food Hygiene and Safety
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• v.9 no.1
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• pp.1-13
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• 1994

A Simultaneous determination method was improved for the determination and confirmation of zeranol, zearalenone, as well as their isomers and metabolites, in beef. The analytes were extracted from tissue by CH3CN, hydrolyzed enzymatically(for glucuronide conjugates), cleaned up by a strong basic anion exchange resin combined with a liquid/liquid partitioning, derivatized using MSTFA and confirmed, quantified by GC/MS/SIM with a internal standard, zearalane. The results were as follows : (1) all the estrogens were separated on the GC/MS chromatogram under the extraction method and the chromatographic conditions improved, the retention times of zearalane-TMS2, zearalanone-TMS2, zearalenone-TMS2, zeranol-TMS3, taleranol-TMS3, and $\alpha$-zearalenol-TMS3, $\beta$-zearalenol-TMS3, were 18.49, 19.44, 19.63, 19.71, 19.79 and 19.99, 20.08 minutes, respectively. (2) The calibration curves of residual zeranol, zearalenone and their metabolites showed constantly linear(r=0.99) in the range of 5~20 ng. The minimum detection concentration of residual zeranol, zearalenone and their metabolites was 1 ppb. (3) The total average recovery of residual zeranol, zearalenone and their metabolites from spiked beef was 60.2%(CV=29.7%) at the 1 ppb and 63.5%(CV=26.5) at the 2 ppb, 72.9%(CV=18.2%) at the 4 ppb. (4) The preservation method for 6 estrogens was improved for the fast running time(21 min) and MSTFA was utilized for derivatizing 6 estrogens for improvement of recovery, for good resolution, for characteristic mass spectra unlike Jose's method and Tina's method. The utilization of zearalane as internal standard showed good quantification result for zeranol, zearalenone, as well as their isomers and metabolites, in beef.

• Analytical Science and Technology
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• v.11 no.1
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• pp.36-41
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• 1998

A gas chromatography-mass spectrometry method for the determination of 5-fluorourasil in human plasma is described. The method involves a single extraction procedure with 10 ml of isopropanol-ether(20:80) solution and pentafluoro-benzylation. Samples were injected using an automatic injector, followed by separation on a nonpolar capillary column and detection with a mass selective detector(MSD). No endogeneous compounds were found to interfere. The detection limit, based upon an assayed plasma volume of 0.5, was 3 ng/ml. The extraction yield was found to be above 80%. Plasma 5-FU concentrations were determined by this method in about 500 plasma samples from cancer patients undergoing treatment with 5-FU. This method is suitable for monitoring of 5-FU in plasma of cancer patients.

• Journal of Food Hygiene and Safety
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• v.29 no.4
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• pp.312-315
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• 2014

The present study demonstrated the development and validation of the method for the quantification of phenol in food using gas chromatography coupled with mass spectrometry (GC-MS). After spiking of internal standard (Phenol-$d_5$) to food, those samples were extracted with organic solvent mixture (acetone : dichloromethane = 1 : 1, v/v) using ultra sonic extractor and cleaned by gel permeation chromatography (GPC) technique. The amount of phenol was determined by GC/MS. To validate the developed method, we evaluated parameters were the selectivity, linearity, accuracy, precision, and recovery. To demonstrate the selectivity of the method, blank samples of rice, corn, and fish(mackerel) were prepared and subjected to GC-MS analysis. To verify the linearity of the method, six different standard concentrations of phenol at 0.01, 0.05, 0.1, 0.5, 1 and 2.5 mg/kg were evaluated. The correlation coefficient ($r^2$) of calibration curve was 0.9999. The recovery rate for phenol standard calculated by internal standard method were 82.2~101.5% for samples fortified with 0.25, 0.50, and 1.0 mg/kg, respectively. Also the repeatability and reproducibility for validation of precision were 0.2~5.5%. According to the result of the validation, this established method was suitable for AOAC guideline. The limit of detection (LOD) for phenol analysis were 0.03~0.1 mg/kg, and the limit of quantification (LOQ) were 0.1~0.3 mg/kg. Therefore, we established the optimal analysis method for determination of phenol in food using GPC and GC/MS.

• Journal of Environmental Health Sciences
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• v.28 no.4
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• pp.27-30
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• 2002

A thermal desorption-gas chromatography/mass spectrometric method was developed for the determination of methyl bromide in fumes formed during preservation of cultural materials from insects. Methyl bromide in lunes was collected by drawing 10ι of air through the adsorbent tube filled with a solid adsorbent (Chromosorb). The air samples were analyzed by using a special thermal desorption device and GC/MS determination. The recovery of methyl bromide by air sampling was 88% and the detection limit of the assay was 0.1 pptv based upon assayed air of 10ι. The method was applied to the determination of fumed methyl bromide used for the preservation of papers in a library. The mean concentration of methyl bromide determined in a library was 280.2 $\pm$ 25.4 pptv.

• Mass Spectrometry Letters
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• v.3 no.1
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• pp.15-17
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• 2012

Eighteen of the PDE-5 inhibitors and their analogues were analyzed using GC-EI-MS. Fourteen of them could be identified by simple GC-MS method without derivatization, but hydroxyhongdenafil, hydroxyvardenafil, xanthoanthrafil and mirodenafil could not be identified without derivatization for the high polarity due to the presence of hydroxyl groups. N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) and N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA), widely used trimethylsilyl (TMS) derivatizing reagents, were used to improve the sensitivity of the hydroxylated analogues. And the analytes could be identified by GC-MS after the derivatization.

• Journal of Environmental Science International
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• v.4 no.3
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• pp.97-97
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• 1995

PCBs have been measured using GC-ECD, GC-MS, GC-ELCD, HPLC, TLC, NMR and Immunoassay. The analysis of PCBs using GC-ECD include the peak pattern method as none derivatization and the Perchlorination method as derivatization. This study was conducted to establish the perchlorination method with Sbcls from PCBs to decachlorinated biphenyl(DCB). The aroclor 1242 of PCBs was chlorinated and then, converted into the DCB which showed a single peak in GC-ECD chromatogram. The detection limit of DCB was 2pg. The quantification detection concentration of PCBs extracted with soxhlet was 0.5ng/g in the soil. PCBs were not detected in the suburban soil, but 174ng/g in the soil of industrial complex. Mean PCBs concentration of Shinchun stream at Kumho river and Jinchun stream at Nakdong river was calculated average 낙ngjg in 각e sediment. PCBs concentration in the sediment of Kumho river near 2-7km from conjunction with Nakdong river was average 154ng/g. PCBs concentration in the sediment of Nakdong river near conjunction with Kumho river was average 159ng/g.

• Journal of Environmental Science International
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• v.4 no.3
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• pp.249-258
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• 1995

PCBs have been measured using GC-ECD, GC-MS, GC-ELCD, HPLC, TLC, NMR and Immunoassay. The analysis of PCBs using GC-ECD include the peak pattern method as none derivatization and the Perchlorination method as derivatization. This study was conducted to establish the perchlorination method with Sbcls from PCBs to decachlorinated biphenyl(DCB). The aroclor 1242 of PCBs was chlorinated and then, converted into the DCB which showed a single peak in GC-ECD chromatogram. The detection limit of DCB was 2pg. The quantification detection concentration of PCBs extracted with soxhlet was 0.5ng/g in the soil. PCBs were not detected in the suburban soil, but 174ng/g in the soil of industrial complex. Mean PCBs concentration of Shinchun stream at Kumho river and Jinchun stream at Nakdong river was calculated average 낙ngjg in 각e sediment. PCBs concentration in the sediment of Kumho river near 2-7km from conjunction with Nakdong river was average 154ng/g. PCBs concentration in the sediment of Nakdong river near conjunction with Kumho river was average 159ng/g.

• Korean Journal of Pharmacognosy
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• v.32 no.3 s.126
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• pp.200-211
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• 2001

This study was carried out to determine the 11 organochlorine, 7 organophosphorus residual pesticides in 251 crude drugs. These residual pesticides in herbal drugs were extracted with acetonitrile and the extracts were cleaned up via LC-florisil solid phase extraction column. The prepared samples were assayed for pesticide residues using GC-ECD, NPD with capillary column and identified by GC-MSD. Recoveries were $63.9{\sim}111.5%$ in the organochlorine pesticides and $69.8{\sim}92.4%$ in the organophosphorus pesticides, and detection limits were $0.001{\sim}0.65\;ppm$ in the organochlorine pesticides and $0.0009{\sim}0.0074\;ppm$ in the organophosphorus pesticides. Pesticide residues were detected in 9 cases.