• 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.

• Analytical Science and Technology
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• v.22 no.3
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• pp.210-218
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• 2009

A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was developed and validated for simultaneous determination of amphetamine derivatives and norketamine in human hair. Preparation of hair involves external decontamination, mechanical pulverization, incubation and extraction prior to instrumental analysis. The samples were derivatized using heptafluorobutyric anhydride, and analyzed by GC-MS/MS. The linear ranges were 0.05-20.0 ng/mg for the analytes except for 3,4-methylenedioxyamphetamine, with good coefficients of determination ($r^2$ >0.998). The intra-day and inter-day precisions were within 10.7% and 8.5%, respectively. The intra-day and inter-day accuracies were between -1.6 and 17.0% and -2.6 and 10.5%, respectively. The limits of detections for each analyte were lower than 0.007 ng/mg, while recoveries were 75.9-100.9%. When the method was applied to hair samples obtained from suspected drug abusers, the concentrations in hair samples were 0.97-19.30 ng/mg for methamphetamine and 0.14-2.56 ng/mg for amphetamine.

• Preventive Nutrition and Food Science
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• v.7 no.1
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• pp.5-11
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• 2002

The comparison of the volatile flavor components from Korean and Japanese Satsuma mandarin (C. unshiu Marcov. forma Miyagawa-wase) peel oils, isolated by cold-pressing, was performed by gas chromatography, mass-spectrometry and gas chromatography-olfactometry (GC-O). Eighty-five volatile components were identified in each oil by GC and GC-MS. Forty-three components were detected in each oil by GC-O. The total amount of monoterpene hydrocarbons was 95.88% (Korean mandarin) and 95.29% (Japanese mandarin). Limonene, ${\gamma}$-terpinene, myrcene and $\alpha$-pinene were the main components of the cold-pressed oils from the both samples. The volatile composition of the Japanese mandarin was characterized by a higher content of sesquiterpene hydrocarbons, especially bicyclogermacrene, $\alpha$-humullene and valencene. The volatile composition of two samples can easily be distinguished by the percentages of aldehydes, ketones and esters, which were found at higher levels in the Japanese mandarin. The sweet and fruity flavor was stronger in the Korean mandarin oil while herbaceous flavor was stronger in Japanese sample. From GC-O data it is suggested that the sweet and fruity flavor of the Korean mandarin resulted from terpinolene and linalool, and the herbaceous note of the Japanese mandarin from $\alpha$-humullene, nepal, ι-carvone and perill aldehyde.

• Korean Journal of Pharmacognosy
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• v.51 no.3
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• pp.207-216
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• 2020

The analysis method for qualitative analysis of the screening method that can be performed prior to the quantitative analysis of individual pesticide was reviewed in order to meet the safety standards that are being strengthened in the field of pesticide residue testing of herbal medicines. Among the residual pesticides presented in the Korean Pharmacopoeia, 56 pesticides, excluding 15 pesticides that need to be individually analyzed, were selected for analysis using QuEChERS preprocessing and GC-MS/MS, which are used in the existing agricultural products field. For each pesticide, the detection limit level of 0.001-0.005 mg/kg and the quantitative limit level of 0.002-0.017 mg/kg were confirmed. In the recovery test in which the standard was treated at a concentration of 0.02 mg/kg, it was confirmed that the proportion of pesticides satisfying the recovery of 70-120% was 85.7-96.4% for each herbal medicine, so it was confirmed that it was a level that could be reviewed by the screening method.

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

• Analytical Science and Technology
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• v.23 no.4
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• pp.395-404
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• 2010

A multi-residual method using gas chromatography coupled with mass spectrometry (GC/MS/ MS) was developed for the analysis of 105 pesticides. This method was tested on lemons, beans and other vegetables. The pretreatment of these pesticides was performed by liquid-liquid partition followed by cleanup with solid phase extraction cartridge (SPE Florisil), after acetonitrile extraction from matrices and sodium chloride (15 g) addition. The recovery ranged from 71.1% to 126.0% except for azinphosmethyl, famoxadone, fenamidone, flufenoxuron and triadimefon in lemons and from 72.5% to 124.5% in bean. In lemon, the limit of detection (LOD) and limit of quantification (LOQ) were 0.001~150 ng/ mL and 0.004~500 ng/mL, respectively.

• Analytical Science and Technology
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• v.34 no.1
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• pp.23-35
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• 2021

In order to measure the volatile organic compounds (VOCs) of a sample which is too large to use commercially available chamber, a stainless steel vacuum chamber (VC) (with an internal diameter of 205 mm and a height of 50 mm) was manufactured and the temperature of the chamber was controlled using an oven. After concentrating the volatiles of the sample in the chamber by helium gas, it was made possible to remove residual volatile substances present in the chamber under reduced pressure ((2 ± 1) × 10-2 mmHg). The chamber was connected to a purge & trap (P&T) using a 6 port valve to concentrate the VOCs, which were analyzed by gas chromatography-mass spectrometry (GC-MS) after thermal desorption (VC-P&T-GC-MS). Using toluene, the toluene recovery rate of this device was 85 ± 2 %, reproducibility was 5 ± 2 %, and the detection limit was 0.01 ng L-1. The method of removing VOCs remaining in the chamber with helium and the method of removing those with reduced pressure was compared using Korean drinking water regulation (KDWR) VOC Mix A (5 μL of 100 ㎍ mL-1) and butylated hydroxytoluene (BHT, 2 μL of 500 ㎍ mL-1). In case of using helium, which requires a large amount of gas and time, reduced pressure ((2 ± 1) × 10-2 mmHg) only during the GC-MS running time, could remove VOCs and BHT to less than 0.1 % of the original injection concentration. As a result of analyzing volatile substances using VC-P&T-GC-MS of six types of cell phone case, BHT was detected in four types and quantitatively analyzed. Maintaining the chamber at reduced pressure during the GC-MS analysis time eliminated memory effect and did not affect the next sample analysis. The volatile substances in a cell phone case were also analyzed by dynamic headspace (HT3) and GC-MS, and the results of the analysis were compared with those of VC-P&T-GC-MS. Considering the chamber volume and sample weight, the VC-P&T configuration was able to collect volatile substances more efficiently than the HT3. The VC-P&T-GC-MS system is believed to be useful for VOCs measurement of inhomogeneous large sample or devices used inside clean rooms.

• Analytical Science and Technology
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• v.19 no.1
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• pp.107-114
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• 2006

Early diagnosis and medical intervention are critical for the treatment of patients with metabolic disorders. A rapid analytical method was developed for simultaneous quantification of organic acids and amino acids in urine without labor-intensive pre-extraction procedure showing high sensitivity and specificity. A new method consisted of simple two-step trimethylsilyl (TMS)-trifluoroacetyl (TFA) derivatization using GC/MS-selective ion monitoring (SIM). Filter paper urine specimens were dried under nitrogen after being fortified with internal standard (tropate) in a mixture of distilled water and methanol. Methyl orange was added to the residue as indicator reagent. Silyl derivative of carboxylic functional group was followed by trifluoroacetyl derivative for amino functional group. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bistrifluoroacetamide were consecutively added and heated for 15-20 min at $65^{\circ}C-70^{\circ}C$, for TMS-TFA derivative, respectively. This reactant was analyzed by GC/MS-SIM. Linear dynamic range showed 0.001-50 mg with the detection limit of (S/N=3) 10-200 ng, and the quantification limit of 80-900 ng in urine. Correlation coefficient of regression line was 0.994-0.998. When the method was applied to the patients 'urine, it clearly differentiated the normal from the patient with metabolic disorder. The study showed that the developed method could be the method of choices in rapid and sensitive screening for organic aciduria and amino acidopathy.

• Analytical Science and Technology
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• v.20 no.6
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• pp.488-495
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• 2007

A wallpaper having many surfaces in indoor is composed of various raw materials. In this study, TVOC contribution from raw materials of PVC wallpaper was evaluated by using headspace-solid phase microextraction (HS-SPME)-GC/MS. Samples were diluent, resin stabilizer, plasticizer, filler, blowing agent and PVC resin. 9 mL of each sample was put into 22 mL glass vial and they were equilibrated for 1 hour at $100^{\circ}C$. Headspace in vial was absorbed to $75{\mu}m$ Carboxen-PDMS fiber and analyzed by GC/MS. Aromatic compounds like a toluene, ethylbenzene and xylene, ketones compounds like a acetone, methoxyacetone and 2-butanone and alkane compounds like a nonane decane and undecane were identified from raw materials. And alcohol compounds like a ethanol and butanol and aldehydes were detected. TVOC emission of diluent, resin stabilizer, plasticizer, PVC resin, blowing agent and filler were $54.20{\mu}g/g$, $32.88{\mu}g/g$, $0.50{\mu}g/g$, $0.88{\mu}g/g$, $0.22{\mu}g/g$ and $0.11{\mu}g/g$, respectively. Contribution of TVOC emission of diluent, resin stabilizer and PVC resin that were concerned about add ratio were 0.708, 0.129, 0.115, respectively. In conclusion, it's necessary to reduce TVOC emission through improvement of diluent, resin stabilizer and PVC resin. Also, HS-SPME-GC/MS method which was developed in this study will be used for raw materials analysis effectively.

• Bulletin of the Korean Chemical Society
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• v.26 no.4
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• pp.575-578
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• 2005

Electrospray ionization mass spectrometry (ESI MS) was used, along with gas chromatography-mass spectrometry (GC-MS), to monitor Paal-Knorr synthesis of 2,5-dimethyl-1-phenylpyrrole by condensation of aniline with 2,5-hexanedione. In addition to 2,5-dimethyl-1-phenylpyrrole observed as a single spot by TLC, unexpected dimer size compounds were observed by GC-MS. Dimers and trimers were observed by ESI MS. ESI tandem mass spectrometry was used to select plausible structures for the dimer. ESI MS with or without liquid chromatographic separation is useful for observing oligomeric byproducts with low volatility produced in organic reactions.