• Bulletin of the Korean Chemical Society
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• 제32권3호
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• pp.977-980
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• 2011

A new analytical method for measurement of 3,4-dihydroxyphenylalanine (DOPA) in human urine was developed. DOPA from an aqueous solution was converted into an ethoxycarbonyl (EOC) derivative. A tertbutyldimethylsilyl (TBDMS) reaction under anhydrous conditions was then attempted for analysis by gas chromatography-mass spectrometry in selected ion monitoring mode. A new mass spectral data on DOPA as a tri-EOC/mono-TBDMS derivative was built. This method showed good linearity (r ${\geq}$ 0.999), precision (% relative standard deviation = 3.1-9.2), and accuracy (% relative error = -7.2-8.8), with a detection limit of 0.05 ng/mL. This selective and accurate method of DOPA analysis will be useful for biochemical monitoring of various neurological disorders including Parkinson's disease in biological fluids.

• Archives of Pharmacal Research
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• 제26권5호
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• pp.416-420
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• 2003

The analytical method of antispasmodic agent tiropramide {$(\pm)\alpha$-(benzoylamino)-4-[2-(diethylamino)ethoxy]-N,N-dipropylbenzenepropanamide hydrochloride} was developed by gas chromatography/nitrogen-phosphorus detector (GC/NPD) in human plasma. Two kinds of tiropramide tablets were orally administered to volunteers by Latin square crossover design, and blood was withdrawn as designed schedule. The plasma of 1 mL was loaded on Sep-pak $C_{18}$ cartridge and eluted with methanol after washing with 30% methanol. The residue dissolved in 100 $\mu$L of methanol after evaporation was analyzed by GC/NPD. Precision (CV%) of intra-day was located within 2.6% and accuracy was less than 9.7%. Inter-day precision was below 8.7% and accuracy was relatively good as less than 14%. Plasma samples obtained from human volunteers were analyzed for the determination of tiropramide concentration by using this method. The method was sensitive, rapid and suitable enough to be applied for pharmacokinetic and bioequivalence studies of tiropramide in human volunteers.

• Bulletin of the Korean Chemical Society
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• 제30권1호
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• pp.61-66
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• 2009

An analytical method based on solid-phase extraction and gas chromatography / mass spectrometry has been developed for measurement of acaricides (amitraz, bromopropylate, coumaphos, cymiazole, and tetradifon) in honey sample. In the stability test of acaricides in honey, amitraz underwent a rapid degradation into 2,4-dimethylaniline (DMA), 2,4-dimethylphenylformamide (DMPF), and N-(2,4-dimethylphenyl)-N'-methylformamidine (DMPMF), whileas other acaricides were found to be stable even for over three months. Extraction of five acaricides from 5g of honey sample was carried out by liquid-liquid extraction using 20mL of ethylacetate. For purification, Florisil-SPE cartridge with elution of 5mL of n-hexane/ acetone (55:45, v/v) was found to remove interferences effectively. Quantification was performed using gas chromatography / mass spectrometry in the selected ion monitoring mode. Spiking experiments were carried out to determine the recovery, precision, and limits of detection (LODs) of the method. The overall recovery values from honey spiked at 0.02 and 0.20 ${\mu}g/g$ levels, respectively, were found to be greater than 75% for all acaricides. The method detection limits for acaricides were ranged from 0.1 to 3 ppb. The developed method in this study was applied for the monitoring of acaricides in honey products collected from urban markets in Korea.

• 대한화학회지
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• 제41권10호
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• pp.524-534
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• 1997

고무가황체는 고분자인 천연고무 및 합성고무에 여러 가지 유기첨가제를 배합하여 만든다. 이와 같은 배합고무의 분석은 여러 가지 다른 성질을 갖는 다양한 첨가제들로 인하여 많은 전처리 과정을 거쳐야 하므로 그 분석이 용이하지 않다. 이를 극복하기 위하여 열분해 가스크로마토그래피질량분석법(Pyrolysis Gas Chromatography-Mass Spectrometry)을 이용하여 고무가황체 중의 유기 고무약품들의 직접분석을 시도하였다. 점착제인 쿠마론-인덴수지(coumarone-indene resin $C-90^{TM}$), 접착제인 알킬페놀 레조시놀 포름알데히드 수지, 가류지연제 등의 고무첨가제의 열분해과정 및 열분해체들의 질량스펙트럼들을 확인하였고 이를 통하여 복잡한 구성 성분으로 이루어진 가황고무 중에서 이들 배합제의 직접분석이 가능하였다.

• 분석과학
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• 제16권1호
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• pp.59-69
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• 2003

Benzophenone (BZP) and 4-nitrotoluene (4-NT) listed as endocrine disrupting chemicals are suspected to contaminate ground water sites and soil. Analytical method for simultaneous determination of the two chemicals in soil and ground water was developed by gas chromatography-mass spectrometry. Water (100 ml) was extracted with hexane, and soil (10 g) was extracted with methanol and hexane. Recovery in water was >72% for BZP and 90-118% for 4-NT. Recovery for 4-NT and BZP in soil was 51-59% with coefficient variation of less than 19.5%. Calibration curves showed a good linearity with $r^2=0.997$. In water and soil collected at nation-wide sites, BZP was found at 5 sites among 43 water sites at the concentration of $14.87{\pm}3.83ng/100 ml$. No 4-NT was found. It is suggested that this method is appropriate to the simultaneous quantitation of 4-NT and BZP in ground water and soil samples.

• 분석과학
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• 제35권5호
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• pp.197-204
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• 2022

A gas chromatography-mass spectrometric method was developed for determining 5-chloro-2-methyl-4-isothiazolin-3-one (CMIT), 2-methyl-4-isothiazolin-3-one (MIT), 1,2-benzisothiazolin-3-one (BIT), 3-iodo-2-propynyl butyl carbamic acid (IPBC) and benzoic acid (BA) in household products. A 0.5 g sample was placed in a test tube and dissolved with 5 mL water, 5 mL methylene chloride and 1.0 mL methanol. The solution was extracted by ultra-sonication followed by mechanical shaking using the salting out effect. Under the established condition, the lowest quantification limits of all analytes were in the range of 0.04-10 mg/kg and their relative standard deviations were less than 8.0 %. The method was used to analyze 10 household products. As a result of analyzing 10 household products, MIT was detected in the range of 1.2-3.5 mg/kg in 3 of 10 samples, CMIT was detected in the range of 2.6-8.2 mg/kg in 3 of 10 samples, and BA was detected in the range of 5.0-15 mg/kg in 4 of 10 samples. Meanwhile, BIT and IPBC were not detected in any of the products. It has been shown that this method can be used for the simultaneous determination of biocides with various physical and chemical properties in household products.

• 한국축산식품학회지
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• 제44권4호
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• pp.934-950
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• 2024

This study addresses the prevalent issue of meat species authentication and adulteration through a chemometrics-based approach, crucial for upholding public health and ensuring a fair marketplace. Volatile compounds were extracted and analyzed using headspace-solid-phase-microextraction-gas chromatography-mass spectrometry. Adulterated meat samples were effectively identified through principal component analysis (PCA) and partial least square-discriminant analysis (PLS-DA). Through variable importance in projection scores and a Random Forest test, 11 key compounds, including nonanal, octanal, hexadecanal, benzaldehyde, 1-octanol, hexanoic acid, heptanoic acid, octanoic acid, and 2-acetylpyrrole for beef, and hexanal and 1-octen-3-ol for pork, were robustly identified as biomarkers. These compounds exhibited a discernible trend in adulterated samples based on adulteration ratios, evident in a heatmap. Notably, lipid degradation compounds strongly influenced meat discrimination. PCA and PLS-DA yielded significant sample separation, with the first two components capturing 80% and 72.1% of total variance, respectively. This technique could be a reliable method for detecting meat adulteration in cooked meat.

• 약학회지
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• 제17권1호
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• pp.41-43
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• 1973

Trace-amounts of Diptered and DDVP in fishes could be separated and identified by thin layer chromatography and gas chromatography with DEGS-H$_{3}$PO$_{4}$ column.

• 한국환경성돌연변이발암원학회지
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• 제21권1호
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• pp.30-33
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• 2001

Salsolinol (1-methyl-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline, SAL), a dopaminergic isoquinoline neurotoxin, has been implicated to contribute the etiology of Parkinson's disease and neuropathology of chronic alcoholism. In our previous results, SAL was reported to have the mutagenicity and clastogenicity not in bacteria but in mammalian cells, and its genotoxic potential was known to be potentiated in the presence of rat liver S-9 fraction. This may indicate that some metabolite(s) of SAL was involved in the mutagenic potentials. To investigate the SAL metabolites, the metabolism studies of SAL were conducted in vitro rat liver S-9 fraction and in vivo using rats by high performance liquid chromatography and gas chromatography/mass spectrometry. The methylated metabolite of SAL was found in urine of rats, while the same methylating form of metabolite was not produced from the in vitro metabolism system using rat liver S-9 fraction.

• 한국작물학회지
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• 제46권4호
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• pp.309-316
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• 2001

Helianthus tuberosus has been known to inhibit the growth of weeds and other plants sharing its habitat. This study was conducted to identify the allelochemicals of Helianthus tuberosus which were extracted with water and solvents. Aqueous extracts of leaf, stem, root, tuber and tuber peel of Helianthus tuberosus except tuber did not show significant differences in phytotoxicity to alfalfa seedlings. It was considered that Helianthus tuberosus contained fewer or less potential water-soluble substances that were toxic to alfalfa. Methanol extract of leaves of Helianthus tuberosus was sequentially partitioned in increasing polarity with n-hexane, ethylacetate and n-butanol. Each extract had a yield of 148, 12, 15.7 and 9.5g, respectively. Inhibitory effects on germination of alfalfa seeds treated with four fractions were not significantly different. But the significant reductions on hypocotyl length were observed for all the solvent extracts. Among the four fractions, the ethylacetate fraction showed the most significant inhibition effect on bioassay with alfalfa. Further separation of the active ethylacetate fraction by open column chromatography led to the 25 subfractions. In bioassay of each sub-fraction with alfalfa seeds, sub-fraction No. 13 showed the most inhibitory effect on seedling growth. $^1$H NMR and gas chromatography-mass spectrometry analysis revealed that sub-fraction No. 13 was the mixture of straight-chain saturated fatty acids.