• Title/Summary/Keyword: HR-GC/MS

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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
    • Proceedings of the Korea Society of Environmental Toocicology Conference
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    • 2003.05a
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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
    • Proceedings of the Korea Society of Environmental Toocicology Conference
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    • 2003.05a
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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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    • v.16 no.5
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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.

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

  • 홍대용;김장락;이장호;문중갑;이한우;김동일;박성학;정주화;이홍근
    • Environmental Analysis Health and Toxicology
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    • v.9 no.1_2
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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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Changes in Physicochemical and Sensory Properties of Hizikia fusiforme Water Extract by Fermentation of Lactic Acid Bacteria (유산균 발효에 의한 톳(Hizikia fusiforme) 추출액의 이화학적 및 관능적 특성 변화)

  • Song, Ho-Su;Kim, Hong-Kil;Min, Hye-Ok;Choi, Jong-Duck;Kim, Young-Mog
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.44 no.2
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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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    • v.9 no.2
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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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Analysis of Physicochemical Characterization and Volatiles in Pure or Refined Olive Oils (국내 유통되는 퓨어 및 정제 올리브유의 이화학적 특성 및 향기 분석)

  • Nam, Ha-Young;Lee, Ju-Woon;Hong, Jang-Hwan;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.36 no.11
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    • pp.1409-1416
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    • 2007
  • Seven selected commercial pure or refined olive oils were obtained from the market, and their physicochemical properties and volatile characterizations were investigated. Fatty acid profiles of the analyzed olive oils showed oleic $(61.2{\sim}74.7mole%)$, palmitic $(10.2{\sim}16.8mole%)$, linoleic $(9.4{\sim}18.0mole%)$, stearic $(1.9{\sim}3.0mole%)$, palmitoleic $(0.7{\sim}2.4mole%)$ and linolenic acid $(0.5{\sim}0.9mole%)$. According to Hunter#s color measurement, pure or refined olive oils showed $L^*$ value of $92.2{\sim}99.0$, $a^*$ value of $-22.2{\sim}-3.2$, and $b^*$ value of $18.5{\sim}55.0$. Their total phenol contents ranged from 1.9 to $13.3mg/100g$ while ${\alpha}-tocopherol$ content showed $7.91{\sim}13.88mg/100g$. Oxidation stability of the pure or refined olive oils were observed by Rancimat. The induction period ranged from 17.37 to 34.72 hr while their POV were $6.83{\sim}20.31meq/kg$ oil. Electronic nose and gas chromatograph-mass spectrometry with head-space solid phase microextraction were applied to identify and discriminate the volatile compounds and flavors in pure or refined olive oils, respectively.

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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    • v.24 no.5
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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.

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

  • Yang, Seung-Ok;Chang, Pahn-Shick;Lee, Jae-Hwan
    • Korean Journal of Food Science and Technology
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    • v.37 no.5
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    • pp.717-722
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    • 2005
  • Formation mechanisms of light-induced volatile compounds were studied using riboflavin-photosensitized oleic acid model systems. Volatile compounds in model systems with 4000 ppm riboflavin at $35^{\circ}C$ under light or in the dark for 39 hr were isolated and identified by a combination of solid phase microextraction (SPME), gas chromatography (GC), and mass spectrometry (MS). Total volatiles in oleic acid with riboflavin under light for 13, 26, and 39 hr increased by 90, 190, and 270%, respectively, compared to those in oleic acid without riboflavin under light. Total volatiles in samples without riboflavin under light or samples with riboflavin in the dark were not significant in tested conditions (p>10.05). Riboflavin did not act as a photosensitizer when it was dispersed in oleic acid. Heptane, octane, heptanal, octanal, nonanal, and 2-nonenal were significantly increased in riboflavin-photosensitized samples compared to those in samples without riboflavin (p<0,05). Light-induced volatile compounds including heptanal and 2-nonenal from oleic acid could be explained using singlet oxygen oxidation, the formation mechanism of which were not understood using triplet oxygen oxidation. These results will help to understand volatile formation in oleic acid containing foods stored under light.

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

  • Chung, Yong-Il;Lee, Ji-Soo;Lee, Hyeon-Gyu
    • Korean Journal of Food Science and Technology
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    • v.41 no.5
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    • pp.522-527
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    • 2009
  • The principal objective of this study was to assess the effects of various manufacturing conditions of soy sauce containing hydrolyzed vegetable protein (HVP) (HVP-soy sauce) on 3-monochloropropane-1,2-diol (3-MCPD) contents. Various HVP soy sauces were prepared under different conditions of alkaline treatment and retention process. Derivatives of heptafluorobutylimidazole (HFBI) 3-MCPD were determined via GC/MS below $0.010{\mu}g/g$, which was sensitive with a good recovery rate. The quantity of 3-MCPD decreased with the pH and temperature of alkaline treatment, and the time and temperature of the retention process increased. Alkaline treatment at pH 10.0-10.5 and a 72 hr retention process were shown to reduce effectively the 3-MCPD contents of HVP-soy sauces. This result indicates that the manufacturing process, particularly alkaline treatment, and retention process would be critical steps in managing 3-MCPD contents in HVP-soy sauce.