• YAKHAK HOEJI
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• v.57 no.6
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• pp.420-425
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• 2013

Phentermine (PT) and phenmetrazine (PM) have been widely used as anti-obesity drugs. These drugs should be used with caution due to its close relation to amphetamine in its structure and toxicity. PT and PM, amphetamine-type anorectics, have recently been considered as alternatives for methamphetamine abuse in Korea. In addition, the misuse and abuse of PT and PM obtained by illegal sources such as the internet become a serious social problem. In the present study, a simultaneous detection and quantification method for determining PT and PM in human urine was developed and validated according to the international guidelines. The urine samples were screened using a fluorescence polarization immunooassay and analyzed by gas chromatography mass spectrometry (GC-MS) after extraction using automatic solid phase extraction (SPE) with a mixed-mode cation exchange cartridge and derivatization with pentafluoropropionic anhydride (PFPA). The validation results for selectivity, linearity, limits of detection (LOD) and quantification (LOQ), intra- and inter-assay precision and accuracy and recovery were satisfactory. The validated method was successfully applied to authentic urine samples collected from 38 drug abuse suspects. PT and/or PM were identified with or without methamphetamine in urine samples. Abuse of PT and PM have increased continuously in Korea, therefore, closer supervision of the inappropriate use of anoretics is necessary.

• Korean Journal of Agricultural Science
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• v.43 no.4
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• pp.634-640
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• 2016

The objective of this study was to evaluate the effectiveness of using HR-GC/MS for the rapid screening of dieldrin residues in soils. Persistent organic pollutants (POPs) of organochlorine pesticides such as dieldrin, were analyzed in sedimentary rock and granite rock collected from greenhouses, Niigata, Japan. Dieldrin remains in Japanese farming soils, more than 40 years after their use as insecticides was prohibited. The averages in soil moisture ranged from 2.79% to 7.20% in soils derived from sedimentary rock and from 25.59% to 31.40% in soils derived from granite rock. Mean concentrations of dieldrin residues in sedimentary rock and granite rock were $39.7ng\;g^{-1}$ and $40.51ng\;g^{-1}$, respectively. Dieldrin residue was detected at a slightly higher concentration in granite rock than sedimentary rock samples. There was no consistency between the two soils or between surface and subsurface soils. The coefficients of variation of the two soils were 10.6% and 8.7%, respectively. These results suggest that our high-resolution mass spectrometry detector (HR-GC/MS) is effective at analyzing residual organochlorine pesticides in soil. In order to increase the precision and sensitivity for chemical analysis of POPs, high-resolution gas chromatography coupled with a HR-GC/MS is highly recommended.

• Analytical Science and Technology
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• v.25 no.1
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• pp.60-68
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• 2012

A gas chromatography-mass spectrometric (GC-MS) method was developed for determining 25 semivolatile organic compounds in water. A 1.0 L water sample was placed in a separatory funnel and saturated with NaCl, and the solution was extracted two times with 40 mL of methylene chloride. Under the established condition, the linear quantification range was 0.02-800 ng/L and the relative standard deviation was less than 15%. The method was used to analyze 16 surface water samples collected from various regions in Gum-River. The samples revealed SVOC concentrations in the range of 0.02-96.8 ng/L. Maximum concentrations of VOCs detected were not exceeded the EPA or Germany guidelines in any of the samples. The developed method may be valuable for monitoring SVOCs in water.

• Journal of the Korean Chemical Society
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• v.41 no.10
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• pp.524-534
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• 1997

Analysis of additives in cured rubber is often a difficult task for analytical chemists because of a wide variety of complex components. Conventional analyses of additives and rubbers have been done in multistep, off-line processes with large sample size and extensive sample preparations. The coumarone-indene resin, resorcinol-formaldehyde resin, and prevulcanization inhibitor have been characterized by their pyrolysis pathways and mass spectra of characteristic pyrolyzates. Pyrolysis Gas Chromatography/Mass Spectrometry (Py-GC/MS) was used in the identification of additives without any sample pretreatment. This result shows that several organic additives in cured rubber can be directly analyzed.

• Journal of the Korean Society of Food Science and Nutrition
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• v.19 no.4
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• pp.311-314
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• 1990

The volatile fraction of Oenanthe stolonifera DC. was extracted by a steam distillation under the atmospheric pressure and analyzed by gas chromatography(GC) and gas chromatogra-phy/mass spectrometry(Gc-MS) The experimental results revealed the presence of 63 volatile components. Among them 39 components identified were composed of 20 hydrocarbonss(61.94%) 9 alcohols(8.76%) 3 ketones(11.5%) 1 ester(1.34%) 1 aldehyde (2.29%) and 5 miscellaneous \ulcorner92.35%) The major volatile components of Oenanthe stolonifera DC. were limo-nene(12.12%) pulegone(94.8%) germacrene D(8.34%) and $\beta$-pinene(7.68%)

• Mass Spectrometry Letters
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• v.3 no.1
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• pp.21-24
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• 2012

$5{\alpha}$-Dihydrotestosterone (DHT) is the primary active metabolite of testosterone, catalyzed by $5{\alpha}$-reductase ($5{\alpha}R$) in the skin, prostate, and liver. In this study, the $5{\alpha}R$ activity in rat liver S9 fraction in the presence of a NADPH-generating system was evaluated and compared by gas chromatography-mass spectrometry (GC-MS)-based in vitro assays. Testosterone and a $5{\alpha}R$ inhibitor, finasteride, were added to the S9 fractions and incubated at $37^{\circ}C$ for 1 h. Both testosterone and DHT were quantitatively measured and compared with two different GC-MS-based steroid profiling techniques. DHT was not detected by conventional GC-MS analysis in the absence of finasteride when the concentration of testosterone in the S9 fraction was less than $0.2{\mu}M$, whereas the isotope-dilution GC-MS (GC-IDMS) system was able to evaluate the $5{\alpha}R$ activity. Because the S9 fraction contains more reactive enzymes and is easier to collect from tissues compared with a microsomal solution, the combination of the S9 fraction and GC-IDMS technique may be a promising assay for evaluating the $5{\alpha}R$ activity in large-scale clinical studies.

• Journal of Microbiology and Biotechnology
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• v.16 no.7
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• pp.1139-1143
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• 2006

Various techniques and strategies have been developed for the identification of intracellular metabolic conditions, and among them, isotope balance-based flux analysis with gas chromatography/mass spectrometry (GC/ MS) has recently become popular. Even though isotope balance-based flux analysis allows a more accurate estimation of intracellular fluxes, its application has been restricted to relatively small metabolic systems because of the limited number of measurable metabolites. In this paper, a strategy for incorporating isotope balance-based flux data obtained for a small network into metabolic flux analysis was examined as a feasible alternative allowing more accurate quantification of intracellular flux distribution in a large metabolic system. To impose GC/MS based data into a large metabolic network and obtain optimum flux distribution profile, data reconciliation procedure was applied. As a result, metabolic flux values of 308 intracellular reactions could be estimated from 29 GC/ MS based fluxes with higher accuracy.

• Environmental Analysis Health and Toxicology
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• v.17 no.1
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• pp.37-51
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• 2002

Eleven phenols including two chlorophenols, eight alkylphenols and bisphenol A were derivatized with isobutylchloroformate to form their isobutoxycarbonyl derivatives. Standard phenol mixture was concentrated for the isobutoxycarbonyl (isoBOC) derivatization and analysed by gas chromatography/mass spectrometry (GC/MS). The recoveries of the derivatization method of alkylphenols, chlorophenols, and bisphenol A were calculated by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison; shaking and heating method. The linear detector responses were obtained in the concentration range of 5∼400 ng, with correlation coefficients varying from 0.9755∼0.9981. Recoveries of the alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison ; the US-EPA method and the isoBOC derivatization method, Eleven phenols in water samples were extracted with dichloromethane and then concentrated. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 85.1∼109.9％ and 90.3∼126.6％ for the US-EPA method and the isoBOC.

• Analytical Science and Technology
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• v.20 no.4
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• pp.315-322
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• 2007

This study has been described the metabolism and excretion in a healthy male urine collected for 24 hr after oral administration of a complex (pseudoephedrine and dextromethorphan). To detect the trace amounts of parent drugs and their metabolites, acid-hydrolyzed urine was extracted and derivatized with MSTFA and MBTFA followed by gas chromatography/mass spectrometric analysis. Two parent drugs and their metabolites were tentatively identified as their derivatives based on the mass spectral interpretation and compared with previous reports. In addition, the time profile of urinary excretion rate for parent drugs and metabolites was studied. On the basis of metabolites identified and excretion rate, the metabolic pathways of both drugs are suggested.

• Food Science of Animal Resources
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• v.34 no.5
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• pp.700-708
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• 2014

The volatile composition of veal has yet to be reported and is one of the important factors determining meat character and quality. To identify the most important aroma compounds in veal from Holstein bull calves fed one of three diets, samples were subjected to solid-phase microextraction (SPME) combined with gas chromatography-quadrupole mass spectrometry (GC-MS). Most of the important odorants were aldehydes and alcohols. For group A (veal calves fed entirely on milk for 90 d before slaughter), the most abundant compound class was the aldehydes (52.231%), while that was alcohols (26.260%) in group C (veal calves fed starter diet for at least 60 d before slaughter). In both classes the absolute percentages of the volatile compounds in veal were different indicating that the veal diet significantly (p<0.05) affected headspace volatile composition in veal as determined by principal component analysis (PCA). Twenty three volatile compounds showed significance by using a partial least-squared discriminate analysis (PLS-DA) (VIP>1). The establishment of the global volatile signature of veal may be a useful tool to define the beef diet that improves the organoleptic characteristics of the meat and consequently impacts both its taste and economic value.