• Mass Spectrometry Letters
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• v.4 no.4
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• pp.75-78
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• 2013

A gas chromatography/mass spectrometric (GC/MS) method was developed as a candidate reference method for the accurate determination of essential fatty acids (linoleic acid, ${\alpha}$- and ${\gamma}$-linolenic acids) in food supplemental oil products. Samples were spiked with three internal standards (stearic acid-$d_{35}$, $^{13}C_{18}$-linoleic acid, and $^{13}C_{18}$-${\alpha}$-linolenic acid). Samples were then subject to saponification, derivatization for methylation, and extraction by organic solvent. For GC/MS measurement, an Agilent HP-88 column, designed for the separation of fatty acid methyl esters, was selected after comparing with other columns as it provided better separation for target analytes. Target analytes and internal standards were detected by selected ion monitoring of molecular ions of their methyl ester forms. The GC/MS method was applied for the measurement of three botanical oils in NIST SRM 3274 (borage oil, evening primrose oil, and flax oil), and measurement results agreed with the certified values. Measurement results for target analytes which have corresponding isotope-labeled analogues as internal standard were calculated based on isotope dilution mass spectrometry (IDMS) approach, and compared with results calculated by using the other two internal standards. Results from the IDMS approach and the typical internal standard approach were in good agreement within their measurement uncertainties. It proves that the developed GC/MS method can provide similar metrological quality with IDMS methods for the measurement of fatty acids in natural oil samples if a proper fatty acid is used as an internal standard.

• Journal of Environmental Health Sciences
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• v.32 no.2 s.89
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• pp.164-170
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• 2006

Ethylene oxide is a genotoxic carcinogen with widespread uses as industrial chemical intermediate and gaseous sterilant. 2-hydroxyethylated N-terminal valine in Hb is a good biomarker for biological monitoring of ethylene oxide exposure, because of its stability. For measuring the hemoglobin adduct formed by exposure of ethylene oxide, we studied the determination of (N-2-hydroxy-ethyl)valine(HEV) in hemoglobin adduct by using GC/MS. Firstly we synthesized HEV with 2-amino-ethanol and bromoisovaleric acid(BIVA) and confirmed it with GC/MS-FID. Its fragmentations were m/z 116(base ion, M+-45) and m/z 130(M+-31). For measuring HEV with higher sensitivity, we use derivatives which were PFPITH(pentafluorophenylisothiocianate) and TBDMS (tributyldimethylsilylation) by using Edman procedure. Its fragmentation were m/z 425(M+-57), m/z 383(M+-99) and m/z 172(M+-310) by using GC/MS. We did biological monitoring for mice inhalation exposure with 400 ppm ethylene oxide. The concentrations of hemoglobin adduct were $168{\pm}3.8\;and\;512{\pm}04$(nmol g-1 globin) at 0.5 hr/day 400 ppm ethylene oxide inhalation exposure group, and $631{\pm}17\;and\;2265{\pm}9.4$(nmol g-1 globin) at 1.0 hr/day 400 ppm ethylene oxide inhalation exposure for 1 and 4 weeks, respectively. We confirmed that (N-2-hydroxy-ethyl)valine(HEV) of hemoglobin was a good biomarker for biomonitoring of ethylene oxide exposure, and can measured with derivatives such as PFPITH(pentafluorophenylisothiocianate) and TBDMS(tributyldimethylsilylation) by using GC/MS.

• Analytical Science and Technology
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• v.15 no.5
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• pp.482-487
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• 2002

International Olympic Committee (IOC) prohibits the use of carteolol which is one of ${\beta}$-blockers. To prove whether carteolol product was taken or not, the analytical method in urine using GC/MS was established, and metabolism and excretion study were evaluated. As compared with acid hydrolysis, enzyme hydrolysis method was more efficiency. Coefficients of variation for intra-assay precision was around 10%. Error was less than 5% except the concentration of $0.05{\mu}g/m{\ell}$. Recovery was 78.5% at $2{\mu}g/m{\ell}$. Free carteolol, conjugated carteolol, and small amount of p-OH carteolol were found in dosed human urine samples. The conjugated form was being 59.4% of the total carteolol in human urine. The amount of carteolol renal excreted for 72 h after oral dose of 10 mg of carteolol was 49% of the administred dose.

• Analytical Science and Technology
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• v.23 no.5
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• pp.477-484
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• 2010

Personal care products are a diverse group of synthetic organic chemicals such as antimicrobial compounds, UV filters and organo-phosphate flame retardants and derived from individual usages of soaps, toothpaste and cosmetics. It has been detected in municipal sewage effluent and various environmental samples such as surface water, marine, soil, sediment and aquatic biota in many countries. The occurrence of personal care products in environmental samples could negatively impact the health of the ecosystem and humans, due to persistent, long-term chronic exposure of aquatic organisms. In this study, fifteen personal care products in aquatic environmental samples were determined by gas chromatography-mass spectrometry (GC-MS) with liquidliquid extraction (LLE). Method detection limits were in the range of $0.004\sim0.273\;{\mu}g/L$. Two compounds (TCEP, TCPP) were detected in surface waters and seven compounds (triclosan, 4-MBC, EHMC, BP-3, TCEP, TPP, TBEP) were detected in sewage treatment plants (STP) influents or effluents.

• Analytical Science and Technology
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• v.13 no.5
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• pp.592-600
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• 2000

The concentration of free fatty acids and fatty acid composition as well as cholesterol supersaturation in bile may be an important factor in the gallstone formation. Therefore, we simultaneously determinded 23 fatty acids in bile by selected ion monitoring (SIM) method of gas chromatography-mass spectrometry (GC-MS). Biliary fatty acids were extracted by aminopropyl column and the extracts with (phospholipid fraction) or without (free fatty acid fraction) alkaline hydrolysis of phospholipid were derivatized with MSTFA/TMCS (N-methyl-N-trimethylsilyl-trifluoroacetamide/trimethylsilylchloride) mixture in order to be detected on the GC-MS. The recovery range of this method was 61.1-99.0% and the RSD value of within-a-day and day-to-day test were 3.1-25.6% and 3.8-27.0%, respectively. Using this method, biliary profile was investigated in the bile of normal controls and patients with gallstones. The amounts and their distribution of free and phospholipid fatty acids showed different pattern between normal subjects and patients.

• Analytical Science and Technology
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• v.13 no.6
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• pp.736-742
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• 2000

The purpose of this study was to determine the homocysteine (Hey), methionine (Met) and cysteine (Cys) using solid phase micro-extraction (SPME)/gas chromatography (GC)-mass spectrometry (MS) in human plasma and to correlate between the plasma concentration of homocysteine with coronary artery disease. The homocysteine, methionine and cysteine in blood can be used as biomarkers for the risk assessment of vascular disease. The plasma homocysteine level for the coronary artery disease patients was higher than general patients. The concentration ranges of the Hcy, Met and Cys for coronary artery disease patients were $18.47-33.38{\mu}mol/L$, $30.16-55.72{\mu}mol/L$ and $183.16-387.32{\mu}mol/L$, respectively. This method showed good sensitivity and convenience.

• Korean Journal of Environment and Ecology
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• v.29 no.4
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• pp.564-569
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• 2015

In order to discover materials that can be used for OLED, extractions of marine microalgae was screened for photoluminescence(PL) properties and analyzed using gas chromatography-mass spectrometry(GC-MS). The extractions of Nitzschia denticula, Navicula cancellata and Nannochloropsis salina showed PL spectroscopy among fourteen marine microalgae species. The selected three fractions from three microalgae were analyzed by GC-MS. According to the results, it was found that the identified organic light-emitting materials can be subdivided into three functional groups based on imidazole, purine and quinoline. These chemicals are considered to have a strong relationship with PL spectroscopy for OLED materials.

• Korean Journal of Food Science and Technology
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• v.29 no.5
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• pp.882-887
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• 1997

Quantitative determination of sulforaphane, S-methylsulfinylbutyl isothiocyanate in 20 cruciferous vegetables of Korean origin was performed. Homogenate of vegetable was extracted with dichloromethane, and the extract, after drying, was subjected to GC/MS analysis, which was based on single ion monitoring (SIM) at m/z 72, 160, 55, 114 and 177. The content of sulforaphane was found to be the highest in the extract of broccoli $(80.2{\sim}617.7\;ppm)$ followed by turnip $(15.4{\sim}23.1\;ppm)$, red cabbage $(9.9{\sim}32.1\;ppm),\;radish\;(5.5{\sim}8.8\;ppm)$ and kale (8 ppm). Among various cultivars of broccoli, broccoli '1243' and broccoli 'Pilgrim' showed higher content of sulforaphane than others. Especially, in the stem of broccoli '1243' and the floret of broccoli 'Pilgrim' the amount of sulforaphane was the highest (>700 ppm). Thus, the content of sulforaphane differed according to the cultivars and the portion of the vegetables.

• Journal of the Korean Chemical Society
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• v.41 no.4
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• pp.186-197
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• 1997

Estrogens, which play an important role in sex hormone and potential inhibitor of cancer cell proliferation were profiled for normal female and male. The nineteen endogeneous estrogens were simultaneously analyzed by selected ion monitoring method of GC/MS. Urinary estrogens were extracted by using Serdolit AD-2 resin, hydrolyzed with $\beta-glucuronidase/arylsulfatase$ from Helix pomatia, liquid-liquid extraction and quantitatively derivatized by MSTFA/TMSCl mixture in order to be detected on the GC/MS. The good quality-control data were obtained through the precision and accuracy test and the recovery range of them was 80.97∼97.81%. The Korean reference values of urinary estrogens were established and differences were found in normal female compared with normal male.

• Analytical Science and Technology
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• v.13 no.1
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• pp.72-80
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• 2000

The HS/GC/MS method was performed to analyze the volatile organic compounds in waste sludge samples. This study was performed to establish the fundamental data by studying the effects of salt, equilibrium temperature and time in the volatile organic compounds analysis. The presence of salts have been found to increase the sensitivity. The peak area is increased from 1.07 to 2.61 times by adding the salts to the water sample, compared with a salt tree sample. The recoveries of target compounds have found between 90% and 127% at sample temperature of $85^{\circ}C$ for 30 min. This HS/GC/MS method can be applied to analyze the volatile organic compounds and organohalo compounds in the environmental matrix.