• The Korean Journal of Pesticide Science
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• v.19 no.4
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• pp.345-353
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• 2015

The aim of this study is to develop residue analysis method for fenoxanil, a MBI (melanin biosynthesis inhibitor) propionamide fungicide, had mainly been used to control rice blast, and disease of other crops, fruits, and vegetables by using GLC/NPD and GC/MS. Extraction with acetone and partition with n-hexane/dichloromethane (80/20, v/v) were performed from hulled rice, soybean, Kimchi cabbage, green pepper, and apple, then column clean-up with florisil was applied. Mean recoveries were 82.2%-109.1% with less than 7.2% of coefficients of variation and limit of quantitation was set at the concentration of 0.04 mg/kg from the five agricultural products through the determination by GLC/NPD equipped with DB-5 capillary column and single laboratory validation. As a confirmatory method, GC/MS selected ion monitoring (SIM) was set from m/z 125.0, 188.9, and 293.0. Developed method is expected to apply the single residue analysis of fenoxanil in agricultural products.

• YAKHAK HOEJI
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• v.46 no.2
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• pp.93-97
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• 2002

Methidathion is one of the organophosphorus pesticides commonly used for stamping out harmful pests in farming areas. This paper presents a fatality due to methidathion intoxication and describes the distribution of methidathion in postmortem blood and tissues obtained at autopsy. Qualitative identification of methidathion was achieved by TLC, GC and GC/MS, and quantitative analysis was performed by GC with thermionic specific detector (TSD). The analytes in postmortem specimens were extracted by liquid-liquid extraction (LLE) with ethylether. After the ethylether layer was evaporated, the residue was partitioned into hexane and acetonitrile, and the acetonitrile layer was used for analysis. Tissue specimens were homogenized with 4% perchloric acid and applied for LLE. After extraction, the extracts were reconstituted 100 $\mu\textrm{g}$ pyraclofos (IS, 100 $\mu\textrm{g}$/ml in methanol) for GC and GC/MS analysis. On analysis of postmortem specimens, methidathion was identified and quantitated. The methidathion concentrations were 2.0 $\mu$l/ml in blood, 24.4 $\mu\textrm{g}$/g in liver, 13.9 $\mu\textrm{g}$/g in lung, 21.8 $\mu\textrm{g}$/g in kidney, respectively.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.24 no.6
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• pp.261-267
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• 2014

In this study, we manufactured melting temperature controllable modified surfur (MS) and studied the properties of sulfur modified cement concrete (SMC). We investigated the effects of sulfur and pyridine content on melting temperature of MS. The reaction is confirmed by measuring Raman spectrophotoscopy. The SMC was produced at Water (W)/Cement (C) = 45 wt%, Sand (S)/Aggregate (A) = 45 wt% and 5, 10, 15 and 20 % of MS on the basis of conventional portland cement, respectively. And then physical properties such as compressive strength, splitting tensile strength and permeability of SMC were measured. As MS added, permeability was decreased, while strength and spalling properties were improved. To confirm the safety of MS and SMC, pyrolyzed gas chromatography (P-GC) and gas hazard test were conducted. The results showed that MS and SMC were relatively safe at an elevated temperature.

• 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.

• Biomolecules & Therapeutics
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• v.15 no.4
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• pp.266-272
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• 2007

A rapid analytical method was developed to quantify very long-chain fatty acids (VLCFAs, C22:0, C24:0, C26:0) in human plasma with good sensitivity and specificity using tert-butyldimethylsilyl (TBDMS) derivatization and stable isotope GC-MS selective ion monitoring (GC-MS/SIM). Two-hundred and fifty ${\mu}L$ of plasma was fortified with deuterated stable isotope internal standards (d3-C22:0, d3-C24:0, d3-C26:0) and standard mixtures of chloroform and methanol, and then extracted with hexane and acetonitrile. To upper layer of liquid-liquid-extraction, N-(t-Butyldimethylsilyl)-N-methyltrifluoroacetamide was added and then heated to $60^{\circ}C$ for 30 min to produce the TBDMS derivatives. Derivatives of VLCFAs were analyzed by GC-MS/SIM. Calibration curves showed a linear relationship for the target compounds in the concentration range of $10^{-4}{\sim}2{\times}10^3\;{\mu}g/mL$ with the correlation coefficient ranging from 0.996 to 0.999. The limit of quantification for the plasma was $10^{-4}{\sim}2{\times}10^{-4}\;{\mu}g/mL$ (S/N=3). When applied to the plasma specimens of patients with peroxisomal disorder, X-linked adrenoleucodystropy (ALD, Mckusick 202370), the method clearly differentiated normal subjects from ALD patients. The C24:0/C22:0 and C26:0/C22:0 ratios were significantly elevated in the plasma of patients with X-linked ALD compared to normal subjects. The new developed method might be useful for a rapid and sensitive diagnosis of X-linked ALD and other peroxisomal disorders.

• 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.