• Biotechnology and Bioprocess Engineering:BBE
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• v.7 no.2
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• pp.76-84
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• 2002

On-line conversion estimation of enzymatic esterification reactions in solvent-free media was investigated. In principle, conversion to ester can be determined from the amount of water produced by the reaction, because water is formed as a by-product in a stoichiometric manner. In this study, we estimated the water production rate only from some measurements of relative humidity and water balances without using any analytical methods. In order to test the performance of the on-line conversion estimation, the lipase-catalyzed esterification of n-capric acid and n-decal alcohol in solvent-free media was performed whilst controlling water activity at various values. The reaction conversions estimated on-line were similar to those determined by offline gas chromatographic analysis. However, when the water activity was controlled at higher values, discrepancies between the estimated conversion values and the measured values became significant. The deviation was found to be due to the inaccurate measurement of the water content in the reaction medium during the initial stages of the reaction. Using a digital filter, we were able to improve the accuracy of the on-line conversion estimation method considerably. Despite the simplicity of this method, the on-line estimated conversions were in good agreement with the off-line measured values.

• Mycobiology
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• v.35 no.1
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• pp.39-43
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• 2007

The antifungal effect of pine needle extract prepared by a distinguishable extraction method and the dry distillation method, was examined. The effect of this extract itself was insignificant. The chemical components of pine needle extract were then investigated by gas chromatographic analysis, and four, chemical components, acetol, furfural, 5-methyl furfural, and terpine4-ol, were identified. The antifungal effects of those four chemical components against Alternaria mali (A. mali), an agent of Alternaria blotch of apple, were then examined. It was observed that the minimum inhibitory concentrations (MICs) were 6.25, 0.78, 0.78, and 12.5 (mg/ml) of acetol, furfural, 5-methyl furfural, and terpine-4-ol, respectively. MICs of furfural and 5-methyl furfural had the same order of magnitude as that of an antifungal agrochemical, chlorothalonil. Although furfural itself can not be completely substituted for an antifungal agrochemical, a partial mixture of furfural and antifungal agrochemical may be used as a substitute. The use of agrochemicals for the prevention of plant disease caused by pathogenic fungus such as A. mali could be partially reduced by the application of this mixture.

• Toxicological Research
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• v.25 no.1
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• pp.41-45
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• 2009

This study was conducted to monitor the level of bifenthrin residues in pear sprayed with 2% bifenthrin wettable powder (WP) at the recommended rate at four different schedules prior to harvest. The target analyte was extracted with acetone, partitioned into dichloromethane, and then purified by florisil chromatographic column. The residue determination was performed on a DB-5 capillary column using GC with electron capture detector (ECD). Linearity of this method was quite good ($r^2$ = 0.9951) in the concentration ranged from 0.2 mg/kg to 10 mg/kg. Recovery test was carried out at two concentration levels, 0.2 mg/kg and 1.0 mg/kg, in three replicates, and their rates were from 82.9% to 107.2%. No quantitative bifenthrin was detected in pear of all kinds of treatments including the treatment sprayed 4 times until 7 days before harvest. This sensitive and selective method can be used to monitor the trace residual amounts of bifenthrin in pear in a quite low concentration level.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.16 no.3
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• pp.222-232
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• 2006

Objectives: The objective of this study was to propose the total isocyanate analytical method which involves derivation of 2,4-toluene diisocyanate(2,4-TDI), 2,6-toluene diisocyanate(2,6-TDI), 4,4'-methylenediphenyl diisocyanate(4,4'-MDI) and 1,6-hexamethylene diisocyanate(1,6-HDI) using 2-chlorobenzyl alcohol(2-CBA) or 2,4-dichlorobenzyl alcohol(2,4-DCBA), and analyzing of hydrolysate of the synthesized urethane with the gas chromatography(GC)/flame ionization detector(FID), GC/pulsed discharge ionization detector-electron capture detector(PD-ECD) and GC/mass selective detector(MSD). Methods: Urethanes were synthesized by reacting 2,4-TDI, 2,6-TDI, 4,4'-MDI and 1,6-HDI to 2-CBA or 2,4-DCBA. Urethanes was verified by TLC, HPLC/UVD and GC/MSD. For field application, the most suitable condition that 2-CBA coated in glass fiber filter removed completely and urethanes were not removed was searched. 2-CBA generated from hydrolysis of urethanes according to hydrolysis conditions. Diisocyanates were collected on field air and analyzed. Results: Urethanes which were white and solid phase synthesized by reacting 2,4-TDI, 2,6-TDI, 4,4'-MDI, 1,6-HDI and 2-CBA or 2,4-DCBA. And urethanes were verified by TLC, HPLC/UVD and GC/MSD. The most suitable conditions to remove 2-CBA coated in glass fiber filter were $87^{\circ}C$ and 20 mmHg and urethanes were not removed under same condition. Hydrolysis yields of urethanes were 99 % to 111 %. 2-CBA, the hydrolysate of urethanes was analyzed by GC/FID, GC/PD-ECD and GC/MSD. Conclusions: Simultaneous analysis of 2,4-TDI, 2,6-TDI, 4,4'-MDI and 1,6-HDI deriving with 2-CBA and 2,4-DCBA, along with a total isocyanate analysis, was feasible with GC/FID, GC/PD-ECD and GC/MSD. This result will be a guide of further study on total isocyanate analysis.

• Journal of Environmental Science International
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• v.15 no.1
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• pp.85-94
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• 2006

The simultaneous analysis of multi-residual pesticides was developed using a gas chromatography (GC) method. In this study, a simple and reliable methodology was improved to detect 154 kinds of pesticides in sinseng extract sample by using a liquid-liquid extraction procedure, open column chromagraphy and chromatographic analysis by CC electron capture detector (ECD) and GC nitrogen-phosphorus detector (NPD). The 154 kinds of pesticides were classified in 4 groups according to the chemical structure. The extraction of pesticides was experimented with $70\%$ acetone and dichloromethane/petroleum ether in order, and cleaned up via open column chromatography $(3\times30cm)$ packed with florisil $(30g,\;130^{\circ}C,\;12hrs)$. The final extract was concentrated in a rotator evaporator at $40^{\circ}C$ until dryness. Then the residue was redissolved to 2ml with acetone, and analyzed by GC-ECD and GC-NPD. The applied concentration of pesticides was over $1\~10{\mu}g/ml$. The recovery tests were ranged from $70.7\%$ to $115.2\%$ with standard deviations between 0.3 and $5.7\%$ of the standard spiked to the ginseng extract sample (Group $I\~IV$). The limit of detection (LOD) ranged from 0.001 to $0.099{\mu}g/ml$ (Group $I\~IV$). The 9 kinds of pesticides were not detected. The developed method was applied satisfactory to the determination of the 154 kinds of pesticides in the ginseng extract with good reproducibility and accuracy.

• Analytical Science and Technology
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• v.33 no.2
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• pp.98-107
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• 2020

Methamphetamine (MA) is currently the most abused illicit drug in Korea. MA is produced by chemical synthesis, and the final target drug that is produced contains small amounts of the precursor chemicals, intermediates, and by-products. To identify and quantify these trace compounds in MA seizures, a practical and feasible approach for conducting chromatographic fingerprinting with a suite of traditional chemometric methods and recently introduced machine learning approaches was examined. This was achieved using gas chromatography (GC) coupled with a flame ionization detector (FID) and mass spectrometry (MS). Following appropriate examination of all the peaks in 71 samples, 166 impurities were selected as the characteristic components. Unsupervised (principal component analysis (PCA), hierarchical cluster analysis (HCA), and K-means clustering) and supervised (partial least squares-discriminant analysis (PLS-DA), orthogonal partial least squares-discriminant analysis (OPLS-DA), support vector machines (SVM), and deep neural network (DNN) with Keras) chemometric techniques were employed for classifying the 71 MA seizures. The results of the PCA, HCA, K-means clustering, PLS-DA, OPLS-DA, SVM, and DNN methods for quality evaluation were in good agreement. However, the tested MA seizures possessed distinct features, such as chirality, cutting agents, and boiling points. The study indicated that the established qualitative and semi-quantitative methods will be practical and useful analytical tools for characterizing trace compounds in illicit MA seizures. Moreover, they will provide a statistical basis for identifying the synthesis route, sources of supply, trafficking routes, and connections between seizures, which will support drug law enforcement agencies in their effort to eliminate organized MA crime.

• Korean Journal of Pharmacognosy
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• v.35 no.4 s.139
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• pp.288-292
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• 2004

To evaluate the quality of the crude drugs using three kinds of Cinnamomum Cortex (CC), Vietnamese CC (VCC, the stem bark of Cinnamomum obtusifolium), periderm-peeled Chinese CC (PPCC, periderm-peeled stem bark of C. cassia), Chinese CC (CCC, stem bark of C. cassia) and a Cinnamomi Ramulus (CR, the twig of C. cassia), the four essential oils were prepared by steam distillation method. Cinnamaldehdye (CAN) and an unknown substance tentatively named hydroxy-cinnamaldehdye(HCNA) were detected in the four essential oils by gas chromatography-mass spectrometry, the contents of which are significantly different one another. Vietnamese CC had the highest content of HCNA whereas CR had the highest CAN content and the lowest HCNA. Vietnamese CC exhibited the greatest cytotoxic activity against the cancer cell lines, A549, HepG-2, HL-60, P-388, U-937, and KB and CR the lowest cytotoxicity. Contents of CAN and HCNA in CCC and PPCC are positioned between VCC and CR. These results suggest that measurement of HCNA and cytotoxicity may determine the quality of CC and CR.

• Journal of Environmental Science International
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• v.22 no.12
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• pp.1539-1549
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• 2013

The purpose of this study is to compare the sampling methods for monitoring indoles (phenol, p-cresol, indole and skatole) in airs of swine facility. As the collecting methods of indoles in air, Tenax-TA adsorption tube and solid phase microextraction (SPME) were examined. For the preparation of calibration curves of indoles concentrated in Tenax-TA, the standard indoles solutions were spiked in each of Tenax-TA tubes and thermally desorbed (ATD) into a gas chromatograph combined with mass detector (GC/MS). And for the preparation of calibration curves by SPME, indoles in the standard gaseous solution prepared by evaporating the aqueous solution that contained indoles into a polyester sampling bag were extracted with SPME fiber and subsequently analyzed by the GC/MS. Two sampling methods were evaluated for extracting indoles present in swine building environments. Results indicated that the SPME method using Polydimethylsiloxane/ Divinylbenzene (PDMS/DVB) fiber was more effective than Tenax-TA method in extracting indoles. The gas chromatographic analysis showed that the linearities of calibration curves and detection limits were useful for detection of indoles in swine airs. The field tests also showed that considerably different levels of indoles were present in various parts of the swine building.

• Journal of the Korean Chemical Society
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• v.8 no.4
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• pp.188-191
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• 1964

A new gas-chromatographic method for determining carbon and hydrogen in organic compounds has been developed. After sample combustion was performed in a regular analytical combustion tube with an internal oxidant (a mixture of silver oxide and manganese dioxide) under a helium flow, the water produced was converted to acetylene by passing through a calcium carbide tube. The carbon dioxide and acetylene were trapped by a molecular sieve 5A column at room temperature. The trapped gases were released under programmed temperature raise up to $340^{\circ}C$ and the released gases were passed through a silica gel column. The adsorption of $CO_2$ and $C_2H_2$ in the molecular sieve 5A trapping column were found to be quantitative and the silica gel column showed an excellent resolution of $CO_2$ and $C_2H_2$ for analytical purpose. The analytical results for various known compounds based on the out-put of the thermal conductivity cell calibrated for the amounts of carbon and hydrogen contents in benzoic acid, showed average errors ${\pm}0.5%$ and ${\pm}0.33%$ for carbon and hydrogen, respectively.

• Food Science and Biotechnology
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• v.17 no.3
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• pp.573-577
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• 2008

$^1H$-Nuclear magnetic resonance (NMR) spectrometry was applied to the quantitative analysis of coumarins in the roots of Angelica gigas without any chromatographic purification. The experiment was performed by the analysis of each singlet germinal methyl, which was well separated in the range of 1.0-2.0 ppm in the $^1H$-NMR spectrum. The quantity of the compounds was calculated by the ratio of the intensity of each compound to the known amount of internal standard (dimethyl terephthalate). These results were compared with the conventional gas chromatography (GC) method. The contents of decursin and decursinol angelate in A. gigas were determined $1.98{\pm}0.07$, $1.13{\pm}0.08%$ in quantitative $^1H$-NMR method and $2.06{\pm}0.24$, $1.17{\pm}0.24%$ in GC method, respectively. The advantages of quantitative $^1H$-NMR analysis are that can be analyzed to identify and quantify, and no reference compounds required for calibration curves. Besides, it allows rapid and simple quantification for coumarins with an analysis time for only 10 min without any preprocessing.