• Archives of Pharmacal Research
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• v.26 no.9
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• pp.697-705
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• 2003

The alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) followed by two work-up methods for comparison: isobutoxycarbonyl (isoBOC) derivatization and tert-butyldimethylsilyl (TBDMS) derivatization. Eleven endocrine disrupting chemicals (EDCs) of phenols in biological samples were extracted with acetonitrile and then the acetonitrile layer underwent freezing filtration 6$0^{\circ}C$ for 2 hours. Solid-phase extraction (SPE) was used with XAD-4 and subsequent conversion to isoBOC or TBDMS derivatives for sensitivity analysis with the GC/MS-SIM mode. For isoBOC derivatization and TBDMS derivatization the recoveries were 92.3∼150.6% and 93.8∼108.3%, the method detection limits (MDLs) of bisphenol A for SIM were 0.062 $\mu$ g/kg and 0.010 $\mu$ g/kg, and the SIM responses were linear with the correlation coefficient varying by 0.9755∼0.9981 and 0.9908∼0.9996, respectively. When these methods were applied to mackerel samples, the concentrations of the 11 phenol EDCs were below the MDL.

• Analytical Science and Technology
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• v.32 no.3
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• pp.88-95
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• 2019

This study was conducted to establish the analytical method for the determination of cyanide in blood, urine, lung and skin tissues in rats. In order to detect or quantify the sodium cyanide in above biological matrixes, it was derivatized to Pentafluorobenzyl cyanide (PFB-CN) using pentafluorobenzyl bromide (PFB-Br) and then reaction substance was analyzed using gas chromatography mass spectrometer (GC/MS)-SIM (selected ion monitoring) mode. The analytical method for cyanide determination was validated with respect to parameters such as selectivity, system suitability, linearity, accuracy and precision. No interference peak was observed for the determination of cyanide in blank samples, zero samples and lower limit of quantification (LLOQ) samples. The lowest limit detection (LOD) for cyanide was $10{\mu}M$. The linear dynamic range was from 10 to $200{\mu}M$ for cyanide with correlation coefficients higher than 0.99. For quality control samples at four different concentrations including LLOQ that were analyzed in quintuplicate, on six separate occasions, the accuracy and precision range from -14.1 % to 14.5% and 2.7 % to 18.3 %, respectively. The GC/MS-based method of analysis established in this study could be applied to the toxicokinetic study of cyanide on biological matrix substrates such as blood, urine, lung and skin tissues.

• Journal of Applied Biological Chemistry
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• v.66
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• pp.144-152
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• 2023

Two different extraction methods were used to evaluate the medical value of common rue, Ruta graveolens L. (RGL). The results of our 2,2-diphenyl-1-picrylhydrazyl and 2,2'-azino-bis-3-ethylbenzothiazoline-6-sulphonic acid assays indicated that the antioxidant activity of RGL essential oil extract obtained through steam distillation was very low, whereas ethanol (EtOH) extracts of RGL showed higher antioxidant activity. RGL essential oil was extracted by steam distillation and characterized by GC/MS analysis. Furthermore, EtOH extracts of RGL were obtained under reflux and analyzed by HPLC/PDA. The GC/MS results indicated that the ketone compounds 2-undecanol acetate, nonyl cyclopropanecarboxylate, and 2-nonanone accounted for more than 70% of the composition of RGL essential oil. The HPLC/PDA analyses indicated that the RGL extracts were rich in phenolic compounds such as protocatechuic acid, rutin, psoralen, xanthotoxin, and bergapten, among which rutin was the most abundant. Collectively, our results demonstrated that RGL contains high levels of phenolic compounds and could thus be commercialized as a valuable plant-derived antioxidant.

• Horticultural Science & Technology
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• v.34 no.1
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• pp.183-194
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• 2016

This experiment was conducted to establish an official determination method to measure fluazinam residue in horticultural crops for import and export using GC-ECD/MS. Fluazinam residue was extracted with acetone from fresh samples of four representative horticultural products, the vegetable crops green pepper and kimchi cabbage, and the fruit crops mandarin and apple. The acetone extract was diluted with saline water and n -hexane partitioning was used to recover fluazinam from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fluazinam was separated and quantitated by GC with ECD using a DB-17 capillary column. The horticultural crops were fortified with three different concentrations of fluazinam. Mean recoveries ranged from 82.5% to 99.9% in the four crops. The coefficients of variation were less than 10.0%. The quantitative limit of fluazinam detection was $0.004mg{\cdot}kg^{-1}$ in the four crop samples. GC/MS with selected-ion monitoring was also used to confirm the suspected residue. This analytical method was reproducible and sensitive enough to measure the residue of fluazinam in horticultural commodities for import and export.

• Journal of the Korean Applied Science and Technology
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• v.34 no.4
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• pp.717-726
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• 2017

The current allowable cross-contamination level of fatty acid methyl esters (FAME) in aviation turbine fuel (AVTUR) is 50 mg/kg, due to that the presence of FAME in AVTUR can significantly impact the fuel supply system and jet engine. It has been difficult to analyze the level of FAME in AVTUR, since it is consisted of a lot of hydrocarbons. In this study, thus, a new method using multi-dimensional GC-MS (MDGC-MS) was proposed in order to determine the FAME level in AVTUR effectively. Applying to MDGC-MS with Deans switching system enabled us to detect and quantify the FAME with low carbon numbers such as those derived from coconut oil and palm kernel oil. The matrix effect of MDGC-MS method, which could shift the FAME peaks to slightly longer retention times, was reduced by 20 times compared with that of 1-dimensional GC-MS reference method. This developed method could be suitable for qualitative and quantitative analyses to determine the contamination level of trace FAME in AVTUR.

• Bulletin of the Korean Chemical Society
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• v.10 no.2
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• pp.196-200
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• 1989

Some s-triazine herbicides, namely simazine, atrazine, and propazine present as trace components in a complex mixture were analyzed by GC/MS and GC/MS/MS methods. Even though monitoring the molecular ions was the best in terms of sensitivity, adequate analysis could not be done when interfering species were present. When doubly charged ions which appeared at characteristic m/z values were monitored, chromatograms were rather free from interference. More importantly, selected reaction monitoring was found to provide a selective means of detection with general applicability.

• Analytical Science and Technology
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• v.29 no.1
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• pp.29-34
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• 2016

This study explores the means by which MX can be effectively extracted from chlorinated water 3-Chloro-4-(dichloromethyl)-5-hydroxy-2(5H)-furanone (MX), a potent mutagen commonly found in chlorinated drinking water at concentrations of up to a few hundred ng/L, was quantitatively determined using sample enrichment followed by liquid-liquid extraction (LLE), derivatization to methylated form, and analysis with GC-MS. A 4-L water sample was enriched to a concentration of 0.4 L using a vacuum rotary evaporator at 30 ℃. MX in the water was extracted using ethyl acetate (100 mL × 2) as a solvent and MX in the extract was methylated with 10 % H₂SO₄ in methanol. MX was recovered at a rate of 73.8 %, which was higher than that (38.1 %) for the resin adsorption method. The limit of quantification and repeatability (as relative standard deviation) were estimated to be 10 ng/L and 2.2 %, respectively. This result suggested that LLE can be used for the determination of MX in chlorinated water as an alternative to more time-consuming resin adsorption method.

• Analytical Science and Technology
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• v.14 no.4
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• pp.300-305
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• 2001

The impurities in isoprene were determined using GC/MS. There were good linearities (above $R^2=0.996$) in the range of the $1.0-50{\mu}g/mL$ and 0.5-5.0%, and the detection limits of the method were below $0.1{\mu}g/mL$ for each impurities. Reagent-grade isoprene contained isopropenyl acetylene and 2-butyne at $10-50{\mu}g/mL$ and the concentrations of cis-piperylene, trans-piperylene, cyclopentadiene and dicyclopentadiene were below $1{\mu}g/mL$. The analysis confirmed that the reagent grade isoprene could be obtained from the distillation of C5 fractions.

• Analytical Science and Technology
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• v.7 no.1
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• pp.65-78
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• 1994

The herbicide mixture of 7 triazines and 9 phenoxyalkanoic acid esters was simultaneously separated and determinated with the selected ion monitoring by using gas chromatography/mass spectrometry. The extraction recoveries of those herbicides from the reagent water were studied for the organic solvent extraction(LLE) with methylene chloride. The calibration curves of them showed good linearity over the concentration range of 0.2~0.5ng/ml and the detection limits were 0.2~0.5ng/ml for 100ml of water. This analytical method could be applied to the drinking water and biological sample.

• Korean Journal of Food Science and Technology
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• v.31 no.5
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• pp.1153-1158
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• 1999

Propolis is a resinous bee-hive product that honeybees collect from plant exudates, flower and leaves. Flavor characteristics of two varieties of propolis collected from different plant origins, falseacacia(Robinia psedoacacia L.) and chestnut tree(Castanea crenata), were analyzed using Aroma Scan and GC/MS. Two varieties of propolis were grouped with quite different aroma profiles by Aroma Scan. Fifty five flavor compounds were identified by GC/MS, of which 44 compounds were found from the propolis of falseacacia and 47 compounds from chestnut tree. Five aldehydes, eight alcohols. five ketones, three esters, one fatty acid, twenty seven hydrocarbons. two terpenes and four phenolic derivatives were identified. Thirty six compounds including benzaldehyde, cinnamyl alcohol, eudesmol and benzyl benzoate were detected in both propolis, eight compounds including geraniol and n-undecane only in propolis of falseacacia and eleven compounds including piperitenone and valencene only in chestnut tree.