• Preventive Nutrition and Food Science
• /
• v.3 no.2
• /
• pp.111-118
• /
• 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.

• YAKHAK HOEJI
• /
• v.37 no.1
• /
• pp.54-65
• /
• 1993

A method for the determination of 16 residual pesticides in crude deugs was examined. Crude drug was extracted with acetonitrile/water solution and the extract was partitioned between hexane/CH$_{2}$Cl$_{2}$ and NaCl saturated water. The organic layer was passed through cleanup column and subjected to the GC/ECD or GC/NPD analysis. Essential oil components in crude drug interfere with the analysis, and sulfuric acid treatment was adapted to overcome this interference.

• Bulletin of the Korean Chemical Society
• /
• v.24 no.1
• /
• pp.27-31
• /
• 2003

A Polythiophene-quinoline/glassy carbon (PTQ/GC) modified electrode was developed for the determination of trace mercury in industrial waste water, natural water, soil, and other media. The electrode was prepared by the cyclic voltammetric polymerization of thiophene and quinoline on glassy carbon (GC) electrode by the potential application from -0.6 V to +2.0 V (50 mV/sec) in a solution of 0.1 M thiophene, quinoline and tetrabutyl ammonium perchlorate (TBAP) in acetonitrile. Optimum thickness of the polymer membrane on the GC electrode was obtained with 20 repeated potential cyclings. The redox behavior of Cu(Ⅱ) and Hg(Ⅱ) were almost identical on this electrode. The addition of 4-(2-pyridylazo)resorcinol (PAR) to the solution containing Cu(Ⅱ) and Hg(Ⅱ) allowed the separation of the components due to the formation of the Cu(Ⅱ)-PAR complex reduced at -0.8V, which was different from the Hg(Ⅱ) reduced at -0.5 V on a saturated calomel electrode (SCE). The calibration graph of Hg(Ⅱ) shows good linear relationship with the correlation factor of 0.9995 and the concentration gradient of 0.33 ㎂/㎠/ppb down to 0.4 ppb Hg. The method developed was successfully applied to the determination of mercury in samples such as river, waste water, and sea water.

• YAKHAK HOEJI
• /
• v.29 no.5
• /
• pp.227-233
• /
• 1985

A new method of determination of fatty acid using gas chromatography-flame photometric detector (GC-FPD) is described. Fatty acid was methylthiomethyl-esterified with methylthiomethy chloride in 1,8-diazabicyclo [5,4,0]-undec-7-ene catalyst and its concentration measured by GC-FPD with 3%OV-1 or 3% FS-1 column. The FPD responses of thirteen fatty acid methylthiomethyl esters were examined and were proportional to the concentration of the esters without regard to their chemical structures. Consequently it was possible to determine various fatty acid using one standard calibration curve by GC-FPD. We could rapidly and conveniently determine varous fatty acids using one standard calibration curve by GC-FPD. We could rapidly and conveniently determine 13 fatty acids in Ginseng Radix alba by this method.

• Bulletin of the Korean Chemical Society
• /
• v.34 no.4
• /
• pp.1065-1069
• /
• 2013

A highly sensitive electrochemical detection method for bisphenol A (BPA) has been developed by using multi-walled carbon nanotube (CNT)-doped titania-Nafion composite modified glassy carbon (GC) electrode. The CNT-titania-Nafion/GC electrode exhibited excellent electrocatalytic activity towards BPA. Therefore, the CNT-titania-Nafion/GC electrode showed improved voltammetric responses for BPA compared to that obtained with bare GC electrode. In addition, cetyltrimethylammonium bromide (CTAB), a cationic surfactant, was added into the BPA sample solution in order to accumulate BPA through hydrophobic interaction between CTAB and BPA. The CNT-titania-Nafion/GC electrode gave a linear response ($r^2$ = 0.999) for BPA from $1.0{\times}10^{-8}$ M to $5.0{\times}10^{-6}$ M with a detection limit of $9.0{\times}10^{-10}$ M (S/N = 3). The modified electrode showed good selectivity against interfering species and also exhibited good reproducibility. The present electrochemical sensor based on the CNT-titania-Nafion/GC electrode was applied to the determination of BPA in food package samples.

• Proceedings of the Korea Society of Environmental Toocicology Conference
• /
• 2004.05a
• /
• pp.73-73
• /
• 2004

• KSBB Journal
• /
• v.30 no.4
• /
• pp.141-147
• /
• 2015

The convenient determination of methylsulfonylmethane (MSM) for a commercially available dietary supplement was developed using gas chromatography (GC)-flame ionization detector (FID). Chromatography was performed on a capillary column ($0.32mm\;I.D{\times}30m$, $0.25{\mu}m$) coated with dimethylpolysiloxane using diethylene glycol methyl ether as an internal standard. The performance characteristics of GC were evaluated in terms of selectivity, linearity, precision, accuracy, recovery, limit of detection (LOD) and limit of quantification (LOQ). The calibration curve was highly linear (the coefficient of determination: 0.9979) within the concentration range of $10.0{\sim}800.0{\mu}g/mL$ for MSM. The recoveries for three fortified concentrations were 96.7~97.1%, 96.6~97.3% and 96.8~97.2%, respectively. The LOD and LOQ of the method were $0.29{\mu}g/mL$ and $0.97{\mu}g/mL$, respectively. All obtained results were acceptable according to the guidelines of the Association of Official Analytical Chemists for dietary supplements. Thus, the validated analytical method using the GC-FID system is suitable for the determination of MSM in dietary supplement formulations for quality control.

• YAKHAK HOEJI
• /
• v.30 no.5
• /
• pp.214-219
• /
• 1986

A gas chromatographic procedure is described for the quantitative analysis of ephedrine hydrochloride, pseudoephediiiie hydrochloride and norephedrine hydrochloride in pharmaceutical preparations. The procedure was based upon the determination of thioureas formed from amines and phenylisothiocyanate. The recoveries of ephedrine, pseudoephedrine and norephedrine from pharmaceutical preparations were 100.7(S.E. 0.9), 99.5(0.8), 99.1(0.8) and 99.1%(O.9), respectively. The high accuracy and precision of this assay were inherent in the flame photometric detectors normally used in gas chromatography.

• Korean Journal of Pharmacognosy
• /
• v.29 no.1
• /
• pp.18-21
• /
• 1998

A method for isolation and quantitative determination of patchouli alcohol from Pogostemonis Herba (Pogostemon cablin) has been developed. Isolation of patchouli alcohol was achieved by column chromatography employing the normal-phase gradient separation system n-hexane-ether on silica gel column. The GC method for quantitative determination of patchouli alcohol provided a method for standardization of the raw drug. It suggested that the average content of patchouli alcohol in Pogostemonis Herba is about 0.26%.

• Bulletin of the Korean Chemical Society
• /
• v.28 no.12
• /
• pp.2293-2298
• /
• 2007

In this study, a dithizone extraction technique involving purge & trap GC-MS was developed for the determination of methylmercury in biological samples, especially blood and fish. After alkaline digestion, methylmercury in biological samples was extracted into dithizone and back-extracted into aqueous sulfide solution. The extracted methylmercury was converted to the volatile ethyl derivative, purged and trapped onto a solid-phase collection medium, and then introduced into the GC-MS system. The determined MDLs of the established method were 0.9 ng·g?1 for biological samples and its accuracy and precision were found to be 93% and 3.8%, respectively. The method was validated by analysis of CRMs such as SRM 966, BCR 463 and IAEA 407 and all analytical results were within certified ranges with average RSDs of less than 6%. The analytical results of field-sampled fish also showed that the method can be successfully used as an alternative for commonly used distillation method followed by GC-CVAFS detection.