• Proceedings of the PSK Conference
• /
• 2003.10b
• /
• pp.241.3-242
• /
• 2003

A simple, specific and sensitive method for the determination of methyltestosterone (MT) in human serum has been developed by gas chromatography/mass spectrometry with the purpose of conducting pharmacokinetic and bioequivalence studies of MT. This method involves the use of liquid-liquid extraction with diethyl ether and derivatization with MSTFA, using 1 ml of serum obtained from volunteers orally taken 50 mg MT. MT showed good resolutions in this conditions and no significant interfering peaks were observed. (omitted)

• Proceedings of the Korean Environmental Sciences Society Conference
• /
• 2003.11a
• /
• pp.113-118
• /
• 2003

An investigation has been carried out on collision-induced dissociation (CID) in the development of an analytical protocol for the determination of polycyclic aromatic hydrocarbons (PARs) by ion trap tandem mass spectrometry. Two different considerations were used to choose the optimal CID conditions for complex matrix environmental samples, namely, to determine the highest signal-to-noise (SIN) ratio and the other to eliminate the background interferences originated from complex matrix samples. The PAR content of agricultural soil was measured to estimate overall distribution of PAR in throughout the country, we collected and analyzed 226 soil samples from paddy and upland soil. The average content of total PAR in all samples was 236 ${\mu}g$ $kg^{-1}$, and the range was from 23.3 to 2, 834 ${\mu}g$ $kg^{-1}$. The overall distribution of PAR was found to be closely related to the pollution sources, the size of city and the type of industry.

• Mass Spectrometry Letters
• /
• v.11 no.4
• /
• pp.103-107
• /
• 2020

We report the application of 2,4,6-trichlorobenzoyl chloride (often referred to as Yamaguchi esterification reagent) for the selective derivatization of the carboxylic group for GC-MS with the sample preparation method optimized for GC-MS analysis. The reagent was shown to be capable of selectively turning the carboxylic group into a reaction center, i.e., anhydride, of which the further reaction was directed to a near complete formation of required esters by unique steric and electronic effects of the reagent. Using the developed method, the chiral separation of hydroxycarboxylic acids by GC-MS using non-chiral columns was successfully demonstrated.

• Korean Journal of Food Science and Technology
• /
• v.20 no.6
• /
• pp.774-779
• /
• 1988

The essential oil of Artemiisa lavandulaefolia DC was analyzed by gas chromatography/mass spectrometry (GC/MS). The oil was stored at different conditions for 6 weeks and the changes of color and chemical composition during storage were checked by GC/MS. The experimental results were as follows; (1) More than 186 chemicals were detected by GC. Major components were 1,8-cineol, thujone, camphor, borneol, coumarin, 2,3-dihydrobenzofuran and ${\beta}-biasbolene$. In this study, 3,3,6-trimethyl norpinanol, ${\beta}-farnesene,\;{\alpha}-curmene$ and 7-methoxy coumarin were detected as new compounds in Artemisia species. (2) It was proved that temperature and/ or light had and important effect on the changes of color and volatile components of the essential oil. The relative amounts of limonene and 1.8-cineol were decreasad, on the other hand, ${\beta}-phellandrene\;and\;{\alpha}-terpineol$ were increased during storage.

• Journal of Environmental Health Sciences
• /
• v.32 no.1 s.88
• /
• pp.67-70
• /
• 2006

A gas chromatography/mass spectrometric method was developed for the determination of formaldehyde in hair. 0.3mg of hair was placed in 10ml headspace vial. 1.5mM pentafluorophenylhydrazine solution (pH 2) in 0.03 M phosphoric acid and $20\;{\mu}l$ of 500 mg/l $acetone-d_6$ as internal standard were added in vial and sealed tightly with cap. The solution was heated for 30 min at $90^{\circ}C$ in heating block. The extraction, the derivatization and the evaporation were performed simultaneously. After heating of the solution, 0.5 ml of headspace was taken up and analyzed by gas chromatography-mass spectrometry (GC-MS). Low limit of detection (LaD) and Low limit of quantitation (LOQ) of formaldehyde were 0.5 and 1.5 ng/g, respectively. The method was used to analyze formaldehyde in rat hair after oral exposure. The developed method may be valuable to be used to analyze formaldehyde in human hair.

• Food Science of Animal Resources
• /
• v.29 no.4
• /
• pp.482-486
• /
• 2009

The aim of this study was to optimize a simple, fast, and economical analysis procedure for the determination of 16 different pesticides in raw milk via GC/MSD. Analyses were performed via gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode (GC/MSD-SIM) using Pentachloronitrobenzene as the internal standard. The modified sample preparation methodology was based on the Pesticide Analytical Manual (PAM) of the FDA concerning fat extraction, ACN-ether partitioning, and clean-up of the Sep-Pak florisil cartridge. The modified methodology for the determination of the 16 pesticides was validated. The range of LOQs of the 16 pesticides was likely three times lower than their Maximum Residence Levels (MRLs). The recoveries of most of the pesticides were acceptable at the fortification levels of 0.5 and 1.0 ${\mu}g/mL$ and their RSD (%) level was less than 20%. None of the 16 pesticides were detected in the selected raw milk samples.

• Analytical Science and Technology
• /
• v.25 no.6
• /
• pp.467-475
• /
• 2012

A gas chromatography-mass spectrometric (GC-MS) method was developed for determining 17 hazard compounds containing phenols, polycyclic aromatic hydrocarbons and pesticides in surface water. A 1.0 L surface water sample was placed in a separatory funnel and saturated with NaCl, and the solution was extracted with 40 mL of methylene chloride. Under the established condition, the lowest quantification limit was 1.0-10 ng/L and the relative standard deviations were less than 22%. The method was used to analyze 70 surface water samples collected from 35 regions in Gum-River. The samples revealed the compounds concentrations in the range of 1.1-26,604 ng/L. Maximum concentrations of compounds detected were not exceeded guidelines established in other countries. The developed method may be valuable for monitoring hazards in water.

• Analytical Science and Technology
• /
• v.13 no.3
• /
• pp.385-393
• /
• 2000

A gas chromatography-mass spectrometric (GC/MS) procedure for the determination of amineptine (dihydro-10, 11-dibenzo[a, d] cycloheptenyl-5-amino-7-heptanoic acid) and its main metabolites in human urine was described. Amineptine has been known to be extensively metabolized by the ${\beta}$-oxidation of the heptanoic side chain with formation of pentanoic side chain metabolite ($C_5$-metabolite), and lactamizarion by internal dehydration of (${\beta}$-oxidized metabolite (${\delta}$-lactam). The detection of these compounds was based on acid hydrolysis, liquid-liquid extraction and trimethylsilylated derivatization of the carboxylic acid group. For the determination of amineptine and its metabolites in biological fluids, selected ions at the m/ 192, molecular ion and one of the characteristic ions were monitored by GC/MS. On the excretion study of amineptine in human urine, 70-90% of amineptine, ${\delta}$-lactam, and $C_5$-metabolite were found to be excreted within 4 hours and their excretion completed within 20 hours.

• Analytical Science and Technology
• /
• v.25 no.1
• /
• pp.60-68
• /
• 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 Pharmaceutical Investigation
• /
• v.39 no.5
• /
• pp.321-325
• /
• 2009

5-HT$_{2C}$ receptors have been considered as therapeutic targets for the treatment of various central nervous system disorders such as depression, anxiety, epilepsy, schizophrenia and sleep disorders. We chemically synthesized KKHQ80114 (K14) and KKHQ80109 (K09), selective 5-HT$_{2C}$ agonists, with the purpose of developing therapeutic agents for the treatment of obesity. The objective of this work is to investigate analytical methods of these compounds in the plasma and urine of rats by gas chromatography/mass spectrometry. In this experiment, K14 was determined in plasma and urine by using K09 as internal standard. Calibration curves give a good linearity in plasma (r$^2$=0.9993) and urine (r$^2$=0.9988). Among hexane, ethyl acetate and diethyl ether, the highest peak was observed in diethyl ether. However, ethyl acetate was used since more interfering peaks were observed with diethyl ether. Inter-day precision and accuracy were determined in the ranges of 50-500 ng/mL for plasma and 10-500 ng/ml for urine. Quantitation limits were 50 ng/mL plasma and 25 ng/ mL urine. These data may be applicable for further studies of these compounds including absorption and metabolism due to no pharmacokinetic or analytical data available.