• 제목/요약/키워드: HR-GC/MS

검색결과 56건 처리시간 0.028초

Identification of urinary metabolite(s) of CKD-712 by gas chromatography/mass spectrometry in rats

  • Jeon, Hee-Kyung;Park, Hae-Yeon;Kim, Youn-Jung;Kwon, Oh-Seung;Ryu, Jae-Chun
    • 한국환경독성학회:학술대회논문집
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    • 한국환경독성학회 2003년도 춘계학술대회
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    • pp.188-188
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    • 2003
  • Examination was made of the urinary metabolite(s) of CKD-712, which is a chiral compound, named S-YS49 derived from higenamine (one component of Aconite spp.) derivatives. First of all, to analyze the metabolite(s) of CKD-712, a simple and sensitive detection method for CKD-712 was developed by using gas chromatography-mass spectrometry GC/MS). Urine was collected from adult male Sprague-Dawley rats 250${\pm}$10g) in metabolic cage for 24hr after oral administration of 100 mg/kg of CKD-712. The recovery of CKD-712 after extraction and concentration with AD-2 resin column was above 90 % from rat urine. The detection limits of CKD-712 in urine was approximately 0.1 ng/mL. It has well been suggested that isoquinoline possessing catechol moiety such as CKD-712 should be subjected to the catechol-O-methyl kransferase activity in vivo. We detected three major peaks of presumed CKD-712 metabolites in the total ion chromatogram obtained from the rat urine sample after oral administration of CKD-712. From these results, it is assumed that the urinary metabolites are mono-methylation in the naphthyl moiety (metabolite I ), methylation at the C-6 or 7 hydroxy group in the isoquinoline moiety and hydroxylation at in the naphthyl moiety (metaboliteII), and methylation at the C-6 or 7 hydroxy group in the isoquinoline moiety (metaboliteIII).

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Kinetic behavior of sophoricoside by gas chromatography/mass spectrometry in rats

  • Jeon, Hee-Kyung;Park, Hae-Yeon;Kim, Youn-Jung;Kim, Youngsoo;Kim, Mi-Kyung;Lee, Seung-Ho;Jung, Sang-Hun;Ryu, Jae-Chun
    • 한국환경독성학회:학술대회논문집
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    • 한국환경독성학회 2003년도 춘계학술대회
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    • pp.189-189
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    • 2003
  • Sophoricoside was isolated as the inhibitor of IL-5 bioactivity from Sophora japonica (Leguminosae). To develope as novel anti-allergic drug, kinetic study was performed in rats. Serum concentration of sophoricoside was measured by gas chromatography-mass spectrometry (GC/MS) in male Sprague-Dawley rat (250${\pm}$10g, n=5) after oral administration of sophoricoside (100mg/kg). The recovery of sophoricoside after extraction and concentration was above 95 % from rat serum. Between-day precision(relative standard deviation 2.2-2.8%) and within-day precision(2.0-12.1%) were determined from replicate analysis of a spiked control and incurred serum sample. The detection limits of sophoricoside in this serum was approximately 0.1 ng/mL. The Pharmacokinetic parameters were derived from the noncompartmental analysis. The C$\_$max/(3.56${\pm}$0.34 $\mu\textrm{g}$/mL) value for sophoricoside in male rat was observed at 7.6 h. The elimination half-life(t$\_$1/2/) of sophoricoside was approximately 4.47 h, the mean residence time (MRT) averaged 10.75 h, the total body clearance (Cl) averaged 0.0042 mL/min/kg. and the area under the serum concentration-time curve (AUC$\_$0-$\infty$/) was 24.93 $\mu\textrm{g}$$.$hr/mL.

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Characteristics and Antioxidative Activity of Volatile Compounds in Heated Garlic (Allium sativum)

  • Woo, Koan-Sik;Yoon, Hyang-Sik;Lee, Youn-Ri;Lee, Jun-Soo;Kim, Dae-Joong;Hong, Jin-Tae;Jeong, Heon-Sang
    • Food Science and Biotechnology
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    • 제16권5호
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    • pp.822-827
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    • 2007
  • The aroma characteristics and antioxidative activity of volatile compounds in heat-treated garlic (Allium sativum L.) were evaluated. The garlic was heated to various temperatures (100, 110, 120, and $130^{\circ}C$) for different lengths of time (1, 2, and 3 hr). The volatile compounds of heated garlic were extracted by simultaneous steam distillation extraction (SDE). Aroma compound profiles were analyzed by gas chromatography/mass spectrometry (GC/MS) and antioxidative activity was measured by 2,2-diphenyl-2-picrylhydrazyl (DPPH) assay and 2,2'-azino-bis-(3-ethylbenzothiazoline-6-sulfonic acid (ABTS) cation decolorization assay. The major aroma compounds were sulfur compounds such as dimethyl disulfide, 2-propen-1-ol, methyl-2-propenyl disulfide, dimethyl trisulfide, diallyl disulfide, methyl-2-propenyl trisulfide, and di-2-propenyl trisulfide. DPPH radical scavenging activity (EDA, %) and the ascorbic acid equivalent antioxidant activity (AEAC) of volatile compounds in heated garlic increased significantly with the increase of temperature and time (p<0.001). The EDA (%) and AEAC of raw garlic were 26.8%/10 mg garlic and 39.05 mg ascorbic acid equivalent per g sample. After heat treatment, the highest values were 40.50%/10 mg garlic for EDA (%) and 46.43 mg ascorbic acid equivalent per g sample for ABTS.

$^{32}$P-postlabelling법을 이용한 유기용제 작업장 근로자의 유전독성 평가 (An Assessment of Genotoxicity on Organic Solvent Workers by $^{32}$P-postlabelling Method)

  • 홍대용;김장락;이장호;문중갑;이한우;김동일;박성학;정주화;이홍근
    • Environmental Analysis Health and Toxicology
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    • 제9권1_2호
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    • pp.37-51
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    • 1994
  • To evaluate the genotoxicities of workers exposed to glue and glue cleaning solution, ambient air monitoring of working place, animal study and human monitoring were carried out. By GC-MS analysis, air samples collected from shoesmaking plant were found to be toluene, xylene, cyclohexane, n-hexane, methyl ethyl ketone, trichloroethylene, butylacetate, isopropyl alcohol. Glue and glue cleaning solution from shoesmaking plant were applicated topically to the CD-1 mice. DNA was isolated from skin 24 hr following the application and analysed for DNA-adducts using the nuclease $P_1$version of $^{32}$P-postlabelling assay. RAL (Relative Adduct Labelling, adducts$10^8$ nucleotides) was significantly increased in a dose-dependent manner in the glue cleaning solution treated mice skin. Peripheral blood DNA-adducts of workers exposed to glue and glue cleaning solution were also analysed by the same method, but there were not significant differences in the peripheral blood DNA-adducts level between exposed and control workers. In addition, glue cleaning solution from shoes factory was evaluated for mutagenicity in the Salmonella plate incorporation assay using strains TA 100 and TA 1535 in the presence and absence of Arochlor 1254-induced rat liver S$_{9}$. There was evident mutagenicity for cleaning solution in TA 100 regardless of $S_9$, but TA 1535 showed positive only in the absence of $S_9$when predicted by Stead model of mutagenicity prediction (p=0.0000). The urine concentrates from workers and controls were also assayed for mutagenicity towards strain TA 100 of Salmonella typhimurium in the presence of $S_9$ using Kado's microsuspension assay, but their mutagenic activities were not found to be significant. These data suggest that shoesmaking workers are exposed to genotoxic compounds and need to be monitored by testing the mutagenicity of human urines. However, $^{32}$P-postlabelling application requires further validation for the routine monitoring of human exposure.osure.

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유산균 발효에 의한 톳(Hizikia fusiforme) 추출액의 이화학적 및 관능적 특성 변화 (Changes in Physicochemical and Sensory Properties of Hizikia fusiforme Water Extract by Fermentation of Lactic Acid Bacteria)

  • 송호수;김홍길;민혜옥;최종덕;김영목
    • 한국수산과학회지
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    • 제44권2호
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    • pp.104-110
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    • 2011
  • This study was conducted to improve the food functional and sensory food quality of Hizikia fusiforme by the fermentation of lactic acid bacteria. Seven strains of lactic acid bacteria isolated from traditional Korean fermented food were inoculated and cultivated in H. fusiforme water extract. Among them, Lactobacillus brevis LB-20, isolated from Kimchi, was selected for further study by considering the results of bacterial growth, DPPH radical scavenging activity, and sensory evaluation. No significant differences in proximate compositions (moisture, crude protein, crude fat, and crude ash) were observed by the fermentation of L. brevis LB-20. The most dramatical change was the conversion from glutamate to ${\gamma}$-aminobutyric acid (GABA) in H. fusiforme water extract fermented by L. brevis LB-20. The GABA content increased approximately 60-fold after 48 hr of fermentation. The bacterial fermentation also resulted in low-molecularization of the extract. The particle size of the fermented extract became approximately 4-fold smaller than that of the law extract. In addition, the analysis of volatile flavor compounds using GC/MS revealed that the bacterial fermentation dramatically removed off-flavors such as acetaldehyde, haxanal, diallyl disulphide and 1-penten-2-ol in the H. fusiforme extract.

Detection of N-Acetyltranylcypromine and Glucuronide of Phenyl-Hydroxylated N-Acetyltranlcypromine from Tranylcypromine-Dosed Rat Urine : Pharmacological Implications

  • Kang, Gun-Il;Choi, Hee-Kyung
    • Archives of Pharmacal Research
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    • 제9권2호
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    • pp.99-110
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    • 1986
  • In order to use for metabolic studies of tranylcypromine (TCP), TCP-phenyl-$d_{5}$ was synthesized via the intermediates, 3-benzoylpropionic acid-$d_{5}$ and trans-2-phenylcyclopropanecarboxylic acid-$d_{5}$ -TCP(0.22 mmole/kg) and its deuterated analog were administered s. c. to the rats and GC/MS analyses of the urines led to the detection of N-acetyltranylcypromine (ATCP) and glucuronide conjugate of phenyl-hydroxylated ATCP. MAO activities in rat brain were measured using serotonin as the substrate. In vitro $IC_{50}$ of ATCP was determined to be $10^{-3}M$. The inhibitions by ATCP were not dependent on the preincubation time and were reversed by washing sedimented mitochondrial pellets after the preincubation. In vivo MAO inhibitions at various times of 0.5, 1.5, 3, 6, 12, and 23 hr after the administration of 0.4 mmole/kg (i. p. ) of ATCP were found to be 0.13, 73, 90, 89, and 74 %, respectively. Similarly, the inhibition percents by 0.015 mmole/kg (i. p. ) of TCP were 94, 99, 95, 91, 71 and 49%. The results strongly suggest that deacetylated product of ATCP may account for its in vivo MAO inhibition. The relationship between the metabolism via phenyl-hydroxylation and the in vivo potency of TCP was examined by QSAR study and it was found that groupings discriminating between the compounds with p-substituents and those without them only ensure high correlations, suggesting that ring-hydroxylation which occurs at the para position in most of the compounds is a determining factor to the potency of TCP.

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국내 유통되는 퓨어 및 정제 올리브유의 이화학적 특성 및 향기 분석 (Analysis of Physicochemical Characterization and Volatiles in Pure or Refined Olive Oils)

  • 남하영;이주운;홍장환;이기택
    • 한국식품영양과학회지
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    • 제36권11호
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    • pp.1409-1416
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    • 2007
  • 국내 시중에서 유통되는 국내외 브랜드의 퓨어 및 정제올리브유에 대한 이화학적 특성 및 이들의 향기 성분을 비교 분석하였다. 총 7종의 퓨어 및 정제 올리브유의 지방산 조성을 비교한 결과 palmitic(16:0, $10.2{\sim}16.8$ mole%), palmitoleic(16:1, $0.7{\sim}2.4$ mole%), stearic(18:0, $1.9{\sim}3.0$ mole%), oleic(18:1, $61.2{\sim}74.7$ mole%), linoleic(18:2, $9.4{\sim}18.0$ mole%) 및 linolenic acid(18:3, $0.5{\sim}0.9$ mole%)로 분석되었다. 색도 분석에서 퓨어 및 정제 올리브유의 $L^*$값은 $92.2{\sim}99.0$, $a^*$값은 $-22.2{\sim}-3.2$, $b^*$값은 $18.5{\sim}55.0$을 나타내었다. 이들의 총 페놀 함량 측정 결과 국내 브랜드 퓨어 올리브유에서는 $2.2{\sim}13.3$ mg/100g, 수입 브랜드 퓨어 및 정제 올리브유에서는 $1.9{\sim}5.1mg/100g$으로 나타났고, ${\alpha}$-토코페롤 함량은 $7.91{\sim}13.88$ mg/100g로 조사되었다. 퓨어 및 정제올리브유 시료들의 초기 POV는 $6.83{\sim}20.31$ meq/kg의 수치를 보였고, 이들의 induction period time은 $17.37{\sim}34.72$ hr로 나타났다. 주요 향 성분의 구별을 위해 SPME-GC/MS 분석을 실시한 결과, 올리브유의 주요 향 성분으로 acetic acid, hexanal, heptanal, 2,4-dimethyl-heptane 등이 동정되었고, MOS 유형의 전자코를 이용하여 퓨어 및 정제 올리브유 향기패턴에 대한 주성분분석을 한 결과, 이들의 원산지별과 국내 수입 브랜드 및 혼합율에 의한 향기 성분 패턴 경향성을 찾아보기 어려웠다.

Studies on the Analysis of Benzo(a)pyrene and Its Metabolites on Biological Samples by Using High Performance Liquid Chromatography/Fluorescence Detection and Gas Chromatography/Mass Spectrometry

  • Lee, Won;Shin, Hye-Seung;Hong, Jee-Eun;Pyo, Hee-Soo;Kim, Yun-Je
    • Bulletin of the Korean Chemical Society
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    • 제24권5호
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    • pp.559-565
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    • 2003
  • An analytical method the determination of benzo(a)pyrene (BaP) and its hydroxylated metabolites, 1-hydroxybenzo(a)pyrene (1-OHBaP), 3-hydroxybenzo(a)pyrene (3-OHBaP), benzo(a)pyrene-4,5-dihydrodiol (4,5-diolBaP) and benzo(a)pyrene-7,8-dihydrodiol (7,8-diolBaP), in rat urine and plasma has been developed by HPLC/FLD and GC/MS. The derivatization with alkyl iodide was employed to improve the resolution and the detection of two mono hydroxylated metabolites, 1-OHBaP and 3-OHBaP, in LC and GC. BaP and its four metabolites in spiked urine were successfully separated by gradient elution on reverse phase ODS $C_{18}$ column (4.6 mm I.D., 100 mm length, particle size 5 ㎛) using a binary mixture of MeOH/H₂O (85/15, v/v) as mobile phase after ethylation at 90 ℃ for 10 min. The extraction recoveries of BaP and its metabolites in spiked samples with liquid-liquid extraction, which was better than solid phase extraction, were in the range of 90.3- 101.6% in n-hexane for urine and 95.7-106.3% in acetone for plasma, respectively. The calibration curves has shown good linearity with the correlation coefficients (R²) varying from 0.992 to 1.000 for urine and from 0.996 to 1.000 for plasma, respectively. The detection limits of all analytes were obtained in the range of 0.01-0.1 ng/mL for urine and 0.1-0.4 ng/mL for plasma, respectively. The metabolites of BaP were excreted as mono hydroxy and dihydrodiol forms after intraperitoneal injection of 20 mg/kg of BaP to rats. The total amounts of BaP and four metabolites excreted in dosed rat urine were 3.79 ng over the 0-96 hr period from adminstration and the excretional recovery was less than 0.065% of the injection amounts of BaP. The proposed method was successfully applied to the determination of BaP and its hydroxylated metabolites in rat urine and plasma for the pharmacokinetic studies.

리보플라빈 광산화에 의한 올레산 모델시스템에서 휘발성 물질 발생연구 (Effects of Riboflavin-photosensitized Oxidation on the Formation of Volatile Compounds in Oleic Acid Model Systems)

  • 양승옥;장판식;이재환
    • 한국식품과학회지
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    • 제37권5호
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    • pp.717-722
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    • 2005
  • 불포화지방산의 대표적인 물질 중 하나인 올레산에 백열등 조사와 리보플라빈에 의해 생성되는 휘발성 물질들을 분리 및 동정하였다. 리보플라빈 첨가 시료에서는 리보플라빈 무첨가 시료 보다 39시간 동안 270%의 휘발성 물질이 더 생성되었으며 수용액형태가 비수용액 시료보다 휘발성 물질이 유의적으로 많이 발생하였다(p<0.05). 2-Heptenal은 리보플라빈 첨가 시료에서만 검출되었으며 heptane, octane, heptanal, octanal, nonanal, 2-nonenal은 리보플라빈 광산화 시료에서 대조구에 비해 39시간 동안 각각 8.71, 5.88, 2.58, 2.16, 2.80, 5.84배 이상 증가하였다. 2-Nonenal과 heptanal과 같이 기존 삼중항산소 산화기작에 의해 설명될 수 없었던 휘발성물질의 생성 기작을 일중항산소에 의한 산화 기작을 통해 제시하였다. 본 연구는 올레산 첨가 식품의 광산화에 의한 휘발성분 profile 규명 자료로 활용될 수 있을 것이다.

3-Monochloropropane-1,2-diol(3-MCPD) 저감화를 위한 아미노산 간장의 제조조건 (Preparation Conditions of Hydrolyzed Vegetable Protein Soy Sauce for the Reduction of 3-Monochloropropane-1,2-Diol (3-MCPD))

  • 정용일;이지수;이현규
    • 한국식품과학회지
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    • 제41권5호
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    • pp.522-527
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    • 2009
  • 본 연구에서는 3-MCPD의 함량을 신뢰할 수 있는 결과값의 도출을 위하여 HFBI 유도체화 방법을 이용하였다. 3-MCPD가 검출되지 않은 양조간장에 3-MCPD를 0.020과 $0.200{\mu}g/mL$의 농도로 spiking하여 그 결과 값을 측정한 결과, 회수율이 95% 이상으로 우수하였으며 분석의 재현성 및 정밀성 또한 우수하였다. 아미노산 간장의 제조 조건 중 3-MCPD의 함량에 영향을 미칠 것으로 추정되는 조건 즉, 알칼리 처리시의 pH와 온도, 그리고 유지 시의 온도와 시간을 다양하게 하여 시료를 제조 한 후, 3-MCPD의 함량을 측정하였다. 그 결과, 알칼리 처리시의 pH와 온도가 높고, 유지 온도와 시간이 증가됨에 따라 3-MCPD의 함량이 감소되는 뚜렷한 경향을 나타내었다. 또한 알칼리 처리 온도와 유지 온도에 대한 영향보다는 알칼리 처리시의 pH가 3-MCPD의 함량에 미치는 영향이 더욱 큰 것으로 판명되었으며, 특히 pH 10.0 이상에서 알칼리 처리를 하였을 경우는 알칼리 처리 온도나 유지시간 및 유지온도 등의 다른 조건들에 상관없이 3-MCPD의 함량이 $0.020{\mu}g/g$ 이하로 현저히 낮아지는 경향을 보였다. 본 연구의 결과에 따르면 일반적인 아미노산 간장의 제조 공정 조건에 변화를 줌으로써 실질적으로 생성되는 3-MCPD의 함량을 현저하게 낮출 수 있음을 알 수 있었으며, 이러한 결과는 아미노산 간장의 3-MCPD 저감화 방안을 강구하기 위한 기초 자료로 활용할 수 있을 것으로 판단된다.