• Journal of the Korean Applied Science and Technology
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• v.22 no.4
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• pp.323-331
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• 2005

Fatty acid compositions of the seed oils of P. schinseng, A. continentalis and A. sessiliflorus, were analyzed by gas chromatography (GC) equipped with a capillary column. A large unusual peak was observed just before the peak corresponding to oleic acid $(cis-9-C_{18:1})$. This unknown fatty acid was isolated by silver ion chromatography and then derivatized into the picolinyl ester. The mass spectrum of the picolinyl ester showed molecular ion at m/z=373 with other diagnostic ions such as m/z=178, 218, 232, 246, 274, 288, 302 and 344. Characteristic absorption peaks at $720\;cm^{-1}$, $1640\;cm^{-1}$ and $3010\;cm^{-1}$ in IR spectrum indicated the presence of cis-configurational double bond in the molecule. The $^1H-NMR$ spectrum of this acid gave two quintets centered at ${\delta}1.638$ (2H, C-3) and ${\delta}1.377$ (2H, C-4), and two multiplets centered at ${\delta}2.022{\sim}2.047$ (2H, C-5) and ${\delta}2.000{\sim}2.022$ (2H, C-8), and multiplet signals of olefinic protons centered at ${\delta}5.3015{\sim}5.3426$ (C-6, J=9.5 Hz) and ${\delta}\;5.3465{\sim}5.3877$ (C-7, J=9.5 Hz). The $^13C-NMR$ spectrum showed 18 carbon resonance signals including an overlapped signal at ${\delta}29.7002$ for C-12 and ${\delta}29.6520$ for C-13 (or they can be reversed), and other highly resolved signals at ${\delta}33.950$, ${\delta}24.558$, ${\delta}26.773$ and ${\delta}27.205$ due to C-2, C-3, C-5 and C-8 of a ${\Delta}^6-octadecenoic$ acid, respectively. From analysis results this unknown fatty acid could be identified as cis-6-octadecenoic acid. The seed oils of P. schinseng and A. sessiliflorus contained petroselinic acid (59.7%, 56.0%), oleic acid (18.3%, 6.1%) and linoleic acid (16.2%, 30.4%) with small amount of palmitic acid (3.0%, 3.1%) while the seed oil of A. continentalis comprised mainly oleic acid (30.2%), petroselinic acid (29.0%), linoleic acid (24.1%) and palmitic acid (13.1%).

• Korean Journal of Environmental Agriculture
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• v.13 no.2
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• pp.199-208
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• 1994

Analytical methods for the determination of the derivatives of the herbicide (${\pm}$)-2-(4-chloro-2-methylphenoxy)propionic acid (MCPP) by capillary column gas chromatography with mass spectrometer (GC-MS) and electron-capture detection (GC-ECD) were studied. A successful procedure was introduced for the ester preparation using $H_2SO_4$, as the catalyst and the alcohol 2,2,2-trichloroethanol (TCE) or 2,2,2-trifluoroethanol (TFE). The identificaiton and elucidation of MCPP by GC-MS spectrometry following the esterification with diazomethane, $BF_3$/methanol, $H_2SO_4$/methanol, TCE, TFE, or pentafluorobenzyl bromide (PFB) were carried out. A comparison of the response-sensitivities among those MCPP esters was made with GC-ECD. Although the methylation product of MCPP was confirmed by GC-MS, its low sensitivity to the ECD limited the detection of MCPP. TCE, TFE, and PFB derivatization methods resulted in a high rate of MCPP esterifications and very sensitive ECD molecular responses. Based on efficiency, convenience, worker safety, and least sample contamination, TFE esterificaiton was considered as the superior method for MCPP analysis to the other methods of derivatization. An accurate method is described for quantifying MCPP in soil leachates by GC-ECD at very low concentrations without the requirement of a complicated clean-up process. As a result, MCPP residues at concentrations of less than $0.1{\mu}g$ in 100ml soil leachate were detected.

• Korean Journal of Food Science and Technology
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• v.37 no.6
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• pp.889-892
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• 2005

Standardized method based on extraction, filtration, and gas chromatography (GC) was developed far propylene glycol analysis to set hygienic norm of safety measure for foods under governmental control. Various columns were tested fur propylene glycol analysis by GC with flame ionization detector. Known amount of propylene glycol was spiked into wheat flour dough and analyzed by developed method. Results showed 101.60% recovery rate for propylene glycol with HP-5 column. Reproducibility test of standards recorded 0.30 for standard variation and 0,42% for relative variation. Using analytical method established, contents of propylene glycol in more than hundred different foods were monitored. Propylene glycol was detected in most foods, indicating propylene glycol is not only commonly added during food preparation, but also is contained naturally in food.

• Journal of the Korean Chemical Society
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• v.42 no.3
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• pp.266-276
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• 1998

Cholesterol supersaturation in bile, which causes gallstone formation, is the result of low bile acid secretion or high cholesterol secretion. The quantitative analysis of cholesterol, bile acids and sterols which are precursors of cholesterol have been used to examine the changes in bile component. We described a simple, sensitive and reproducible method for simultaneous determination of cholesterol, five bile acids and seven sterols in human bile juices and gallstones by capillary column gas chromatography-mass spectrometry (GC/MS). Clinical samples were hydrolyzed by alcoholic KOH, extracted twice (pH 14 and 1) and derivatized to trimethylsilyl (TMS) ether with $MSTFA/NH_4I$ (N-methyl-N-trimethylsilyltrifluoroacetamide/ammonium iodide) mixture in order to be detected on the GC/MS. The good quality control data were obtained through within-a-day and day-to-day test (RSD values were 1.72-13.79, 0.68-14.10, respectively) and the recovery range of them was 73.56-96. 95 Using this method, biliary and gallstone compositions in the patients with intrahepatic stones were analyzed. The amounts and its relative distribution of cholesterol, bile acids and sterols showed different pattern in bile juices and gallstones.

• 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.

• Applied Chemistry for Engineering
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• v.18 no.6
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• pp.643-649
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• 2007

Lipase-catalyzed esterification of structural butanol isomers and n-butyric acid was investigated in supercritical carbon dioxide. The experiments were performed in a high pressure cell for 5 hrs with a stirring rate of 150 rpm at 323.15 K and 130 bar. The Candida Antarctica lipase B (CALB) was used in whole system as a catalyst. The experimental results were analyzed by GC-FID using a INNOWax capillary column. The conversion yield and the tendency of the esterification in supercritical carbon dioxide were compared with estimated results by molecular dynamics simulation. Based on the Ping-Pong Bi-Bi mechanism with competitive inhibition, each step of the reaction was optimized; using this result the transition state was predicted. Conformational preference of isomers was also analyzed using molecular dynamics simulations. This kind of approach will be further extended to the prediction of enzyme-catalyzed reactions using computers.

• Korean Journal of Food Science and Technology
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• v.30 no.1
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• pp.6-12
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• 1998

Degummed and bleached soybean oil was deodorized at a temperature range of $220{\sim}280^{\circ}C$ under the vacuum (4-5 torr) for 1 or 2 hrs. Gas chromatography with SP-2560 100 m capillary column was used to separate and quantitate fatty acid methyl esters and their isomers. Fatty acids were identified by comparing retention time with standards and GC-MS spectrum. The isomers of linoleic acid and linolenic acid in deodorized soybean oils were identified to be $C_{18:2}\;{\Delta}9-cis,\;{\Delta}12-trans,\;C_{18:2}\;{\Delta}9-trans,\;{\Delta}12-cis,\;C_{18:2}\;{\Delta}9-cis,\;{\Delta}12-cis,\;C_{18:3}\;{\Delta}9-cis,\;{\Delta}12-cis,\;{\Delta}15-trans,\;C_{18:3}\;{\Delta}9-trans,\;{\Delta}12-cis,\;{\Delta}15-cis,\;C_{18:3}\;{\Delta}9-cis,\;{\Delta}12-trans,\;{\Delta}15-cis,\;and\;C_{18:3}\;{\Delta}9-cis,\;{\Delta}12-cis,\;{\Delta}15-cis$. The formation of trans-fatty acids by deodorization at $240{\sim}280^{\circ}C$ for 2 hrs was in the range of 1.78 to 5.74%. Conclusively, the deodorizing conditions of $240^{\circ}C$ for 2 hrs or $250^{\circ}C$ for 1 hr were suggested as the best conditions which could minimize the formation of trans isomers of fatty acids in soybean oils.

• Analytical Science and Technology
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• v.19 no.2
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• pp.155-162
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• 2006

In this study, a series of experiments were conducted using a standard solution containing ${\alpha}$ and ${\beta}$-endosulfan to follow the removal effect of residual pesticides on soil and aqueous solution. An analytical method for residual pesticides was established by a gas chromatography equipped Ultra II[$(30m{\times}0.25mm(ID){\times}0.25{\mu}m$] capillary column and a ${\mu}$-electron capture detector(${\mu}$-ECD). Recovery rates of residual pesticides for soil samples were 96-100%. The amount of ${\alpha}$ and ${\beta}$-endosulfan that was spread in the soil was checked for various period of time. It indicated that the amount was reduced to 73 and 61%, respectively. When the water spread amount increased from 10 to 100 mL, ${\alpha}$-endosulfan was eliminated from 45 to 85% and while ${\beta}$-endosulfan from 44 to 88%. Removal rates of ${\alpha}$-endosulfan and ${\beta}$-endosulfan were 99% and 98% respectively within 30 minutes. It was assumed that the organic salts and strong alkali elements contained in the pesticide degradator hydrolyzed the residual pesticide.

• Korean Journal of Food Science and Technology
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• v.45 no.5
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• pp.531-536
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• 2013

We developed a simple, sensitive, and specific analytical method for prometryn using gas chromatography-mass spectrometry (GC-MS). Prometryn is a selective herbicide used for the control of annual grasses and broadleaf weeds in cotton and celery crops. On the basis of high specificity, sensitivity, and reproducibility, combined with simple analytical operation, we propose that our newly developed method is suitable for use as a Ministry of Food and Drug Safety (MFDS, Korea) official method in the routine analysis of individual pesticide residues. Further, the method is applicable in clams. The separation condition for GC-MS was optimized by using a DB-5MS capillary column ($30m{\times}0.25mm$, 0.25 ${\mu}m$) with helium as the carrier gas, at a flow rate of 0.9 mL/min. We achieved high linearity over the concentration range 0.02-0.5 mg/L (correlation coefficient, $r^2$ >0.998). Our method is specific and sensitive, and has a quantitation limit of 0.04 mg/kg. The average recovery in clams ranged from 84.0% to 98.0%. The reproducibility of measurements expressed as the coefficient of variation (CV%) ranged from 3.0% to 7.1%. Our analytical procedure showed high accuracy and acceptable sensitivity regarding the analytical requirements for prometryn in fishery products. Finally, we successfully applied our method to the determination of residue levels in fishery products, and showed that none of the analyzed samples contained detectable amounts of residues.

• Korean Journal of Food Science and Technology
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• v.42 no.4
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• pp.383-389
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• 2010

The aim of this study was to determine the methylmercury (MeHg) levels in abyssal fish species. The MeHg in the fishes was extracted with hydrochloric acid and toluene and then purified using an L-cysteine solution. The extract was analyzed with a gas chromatography-electron capture detector (GC-${\mu}ECD$) with a thermon Hg-capillary column. The detection limit and the recovery of the method were 0.002 and 84.2-98.5% (mean, 93.4%), respectively. The MeHg content in 492 abyssal fishes ranged from 0.037 to 2.009 mg/kg. The levels of MeHg [range, mg/kg (mean)] were significantly dependent on fish species and presented as the following; 0.157-2.009 (0.546) in Scalloped hammerhead shark, 0.211-0.878 (0.501) in Blue shark, 0.121-0.993 (0.482) in Spiny dogfish, 0.243-0.658 (0.397) in Salmon shark, 0.074-1.958 (0.353) in Blacktip shark, 0.038-0.807 (0.302) in Southern hake, 0.099-0.511 (0.300) in Scorpion fish, and 0.037-0.133 (0.067) in Ling. The monitoring results showed that the estimated weekly intake of MeHg from sharks, Southern hake, and Ling were lower than the provisional tolerable weekly intake recommended by the Joint FAO/WHO expert committee on food additives.