• 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.

• Bulletin of the Korean Chemical Society
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• v.28 no.12
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• pp.2293-2298
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• 2007

In this study, a dithizone extraction technique involving purge & trap GC-MS was developed for the determination of methylmercury in biological samples, especially blood and fish. After alkaline digestion, methylmercury in biological samples was extracted into dithizone and back-extracted into aqueous sulfide solution. The extracted methylmercury was converted to the volatile ethyl derivative, purged and trapped onto a solid-phase collection medium, and then introduced into the GC-MS system. The determined MDLs of the established method were 0.9 ng·g?1 for biological samples and its accuracy and precision were found to be 93% and 3.8%, respectively. The method was validated by analysis of CRMs such as SRM 966, BCR 463 and IAEA 407 and all analytical results were within certified ranges with average RSDs of less than 6%. The analytical results of field-sampled fish also showed that the method can be successfully used as an alternative for commonly used distillation method followed by GC-CVAFS detection.

• Korean Journal of Food Science and Technology
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• v.35 no.4
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• pp.648-652
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• 2003

Precise and rapid method out for distinguishing blended sesame oils through the electronic nose analysis was developed. Sesame oil was blended with corn oil at the ratio of 95 : 5, 90: 10, and 80 : 20 (w/w), respectively. Samples were then analyzed by gas chromatography, SPME-GC/MS, and the electronic nose composed of 12 different metal oxide sensors. Sensitivities $(delta\;R_{gas}/R_{air})$ of sensors from electronic nose were analyzed by principal component analysis (PCA). Proportion of the first principal component was 98.76%.

• Korean Journal of Food Science and Technology
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• v.45 no.5
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• pp.537-544
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• 2013

This study was performed to establish method of simultaneous determination of fructose, glucose, and sucrose in honey and commercial vitamin drinks by GC and GC/MS. Optimum chromatographic separation of trimethylsilyl-oxime (TMSO) derivatives by GC was achieved on a DB-5 column. Calibration curves for fructose, glucose and sucrose TMSO derivatives by GC were linear in the range of 50-5000 ${\mu}g/mL$, and their $r^2$ values were 0.9999, The limit of detection and limit of quantification of fructose, glucose, and sucrose were 0.68, 0.47, and 0.53 ${\mu}g/mL$, respectively, and 2.27, 1.58, and 1.77 ${\mu}g/mL$, respectively. Average recoveries of fructose, glucose, and sucrose were 100.5, 101.0, and 99.7%, respectively. When the method was applied to 12 honey samples, the average concentrations of fructose, glucose and sucrose were $42.58{\pm}1.97%$, $27.74{\pm}1.16%$, and $0.79{\pm}0.52%$, respectively. The F/G ratio was $1.53{\pm}0.07$. For fructose and glucose contents, results from the GC analysis were similar to those from the HPLC analysis, but the sucrose content was different for each analysis method. We suggest that the GC method is more suitable than other official analytical methods for simultaneous determination of fructose, glucose, and sucrose in honey.

• Journal of the Korean Chemical Society
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• v.48 no.1
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• pp.17-27
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• 2004

A procedure based on solid phase microextraction extraction(SPME)-GC/MS has been developed for the simultaneous analysis of plasticizers. The plasticizers investigated in this study are dimethyl phthalate(DMP), diethyl phthalate(DEP), dibutyl phthalate(DBP), benzylbutyl phthalate(BBP), diethylhexyl phthalate (DEHP), di-n-octyl phthalate(DnOP). The limit of detection(LOD) was 0.163~0.299 with relative standard deciation(RSD) of 5.85~15.80% for these compounds. At water reserviors of Han, Geum, Nakdong and Sumjin rivers, only DBPand DEHP were detected at trace level, 0.192~1.270 ng/ml for DBP and 0.077~1.102 ng/ml for DEHP depending on the river.

• Journal of the Korean Society of Food Science and Nutrition
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• v.26 no.2
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• pp.209-213
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• 1997

Since Houttuynia cordata is well known as a medicinal herb, due to its antibacterial activity on various microorganisms, present investigation was performed to identify the flavor compounds for volatile essential oil. Volatile essential oil was collected by simultaneous distillation-extraction(SDE), and then the oil components were separated on HP-5 capilliary column$(25m{\times}0.25mm\; i.d.)$ and identified those components by GC-MS. Fifty two compounds were isolated from the volatile essential oil of Houttuynia cordata and forty four were positively identified by GC-MS. The volatile compounds were composed mainly of terpenoids(25 classes), aldehydes(7 classes), alcohols(4 classes), ketones(3 classes), acids(1 class) and miscellaneous compounds(4 classes). Of these, the major compounds were ${\beta}-myrcene$, ${\beta}-ocimene$, decanal, 2-undecanone and geranyl propionate.

• YAKHAK HOEJI
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• v.54 no.6
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• pp.429-440
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• 2010

HS-SPME-GC/MS was studied and optimized for the determination of 17 orgarnophosphorous pesiticides (OPPs: chlorpyrifos, chlorpyrifos-methyl, demeton-s-methyl, diazinon, dimethoate, EPN, fenitrothion, fenthion, malathion, methidathion, monocrotophos, parathion, phenthoate, phosphamidon, sulfotep, terbufos, triazophos) in blood. Optimum SPME parameters were selected: choice of SPME fiber (85 ${\mu}m$ polyacrylate), pH effect (0.5 N HCl), salt effect ($Na_2SO_4$, 0.2 g; 20%), headspace incubation temperature ($80^{\circ}C$), headspace incubation time (1 min), headspace adsorption time (30 min) and GC desorption time (2 min). These parameters were optimized using HS-SPME autosampler coupled with gas chromatography-mass spectrometry (GC-MS). Method validation was carried out in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ) and recovery in blood. The assay was linear over 0.5~5.0 mg/l ($r^2$=0.955~1.000). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.03~0.3 mg/l (S/N=3) and 0.1~1.1 mg/l (S/N=10), respectively. Relative recovery with 0.5, 1 and 5 mg/l (in blood) were 90.8%, 98.5% and 94.1%, respectively. This method will be applied to the determination of the orgarnophosphorous pesticides in postmortem blood. The proposed protocol can be an attractive alternative to be used in routine toxicological analysis.

• Applied Biological Chemistry
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• v.39 no.6
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• pp.517-520
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• 1996

To identify the volatiles of Platycodon roots, the three-year-old and the 24-year-old Platycodon roots cultivated in a local farm were extracted with ethyl ether by SDE method. 54.71mg% and 80.01mg% of volatile components were collected in the three-year-old and in 24-year-old Platycodon roots, respectively. As a result of GC/MS(TIC) analysis, 24 and 28 compounds were identified, respectively; The amounts of volatile components such as hexanol, trans-2-hexenol and nonanal in 24-year-old roots were detected above ten times than those in 3-year-old roots. The Volatiles of 24-year-old roots were fractionated by SCC and identified by GC/MS to be 10 hydrocarbons, 8 alcohols, 10 aldehydes, 5 esters, 6 acids and 1 unknown compound as the major components. The species and total amounts of volatile component in 24-year-old Platycodon roots were considered to be higher than those in 3-year-old Platycodon roots. *Abbreviations 1. Platycodon : platycodon grandiflorus (jacquin) A. De Candolle. 2. SDE : Simultaneous Distillation Extraction 3. SCC : Silicagel Column Chromatography 4. GC : gas chromatography 5. GC/MS : Gas Chromatography-Mass Spectrometer 6. TIC : Total Ion Chromatogoraphy

• Analytical Science and Technology
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• v.24 no.3
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• pp.183-192
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• 2011

This study was done for the determination and excretion profile of superdrol and its metabolites in human urine using both liquid chromatography with electrospray ionization mass spectrometry and gas chromatography with mass spectrometry after trimethylsilylation. Superdrol and its two metabolites were detected in human urine after administration of superdrol to healthy volunteers. The intra-day recovery ranged 89.7-113.2%, accuracy ranged 91.8-113.8% and reproducibility ranged 0.2-6.8% and inter-day recovery ranged 89.3-104.1%, accuracy ranged 95.2-103.0%, reproducibility ranged 0.7-7.8%. We found that superdrol M1 was a hydration at C-3 and superdrol M2 was a hydroxylation at D-ring. Superdrol and two metabolites were excreted as their glucuronided fractions. The glucuro-/sulfa-conjugated ratio of superdrol, superdrol M1 and superdrol M2 were 0.02, 0.02, 0.01, respectively. The excretion studies showed that superdrol and two metabolites were reached 4.3 h after oral administration and superdrol and superdrol M1 were detected until 48 h in human urine.

• Korean Journal of Agricultural Science
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• v.38 no.4
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• pp.723-730
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• 2011

To search for the new development of industrial application of woody plants, the chemical composition of the volatile constituents from woody plants (Evodia daniellii, Clerodendron trichotomum, Prunus padus, and Zanthoxylum ailanthoides) was determined by GC and GC/MS spectrometric analysis with the aid of NBS, Wiley Library and RI indice searches. The major constituents were t-ocimene from the leaves of E. daniellii, linalool from the leaves of C. trichotomum, benzaldehyde from the leaves and twigs of P. padus, ${\beta}$-thujene from the leaves of Z. ailanthoides, and 2-undecanone from the stems of Z. ailanthoides. These results suggested that the major volatile constituents of woody plants could be a useful lead compound in the development of functional materials for industrial application.