• Applied Biological Chemistry
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• v.45 no.2
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• pp.101-107
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• 2002

The essential oils isolated from leaves, flowers, stems, and fruits of Vitex rotundifolia by steam distillation and extraction (SDE) method were analyzed by gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS). A total of 76 components detected by GC, 42 components were identified positively by GC-MS and GC co-injection with authentic standards, and 34 components were identified tentatively by mass spectral data only. They included 16 monoterpene hydrocarbons, 30 oxygenated hydrocarbons, 10 sesquiterpene hydrocarbons, 8 oxygenated sesquiterpenes, 3 diterpenes, and 9 miscellaneous components. The major components in the oil from the leaves were ${\alpha}-pinene$ (30.25%), 1,8-cineole (19.89%), sabinene (9.56%), ${\alpha}-terpineol$ (7.94%), ${\beta}-pinene$ (5.69%), and terpinen-4-ol (2.37%), and those in the flower oil were ${\alpha}-pinene$ (25.47%), 1,8-cineole (7.69%), manoyl oxide (6.21%), ${\beta}-pinene$ (4.20%), ${\alpha}-te.pineol$ (3.76%), and sabinene (2.78%). The major components in the oil from the stems were ${\alpha}-pinene$ (13.24%), ${\alpha}-terpineol$ (10.64%), 1,8-cineole (4.40%), manoyl oxide (4.02%), ${\beta}-pinene$ (2.39%), and terpinen-4-ol (2.21%) while those in the oil from the fruits were ${\alpha}-pinene$ (20.24%), 1,8-cineole (11.47%), ${\beta}P-pinene$ (9.79%), ${\alpha}-terpineol$ (7.08%), sabinene (3.68%), and limonene (2.77%). The percentage composition of monoterpenes in the oils from the leaves and the fruits were higher than in those from the flowers and the stems, whereas the oil from the flowers and the stems were characterized by a large content of sesquiterpenes, diterpenes and other unknown high molecular weight components.

• Korean Journal of Medicinal Crop Science
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• v.2 no.3
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• pp.234-240
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• 1994

The essential oils of Thymus quinquecostatus Celakov. and T. magnus Nakai, respectively, were isolated by using a modified Likens-Nickerson type steam distillation and extraction apparatus and analyzed by gas chromatography and gas chromatography-mass spectrometry. The oil content of T. quinquecostatus was 1.94%, and that of T. magnus was 1.91% in mixed leaves and stems and 0.68% in flowers. Among 38 components identified in either mixed leaves and stems or flowers the major components in essential oil isolated from T. quinquecostatus were thymol(39.8%), ${\gamma}-terpinene(10.0%)$ ${\rho}cymene(9.2%)$ and camphor(5.9%) while those from mixed leaves and stems of T. magnus were thymoI(54.7%), ${\gamma}-terpinene(15.8%)$, ${\rho}cymene(6.7%)$ and carvacroI(3.2%). The contents of ${\alpha}-pinene$, camphene, camphor, bornyl acetate and ${\alpha}-terpinene+borneol$ were higher in T. quinquecostatus than in T. maglnus but ${\gamma}-terpinene$ and thymol were higher in T. magnus than in T. quinquecostatus. Comparing leaves and stems with flowers in T. magnus, peak area percentage(%) of ${\gamma}-terpinene$, ${\alpha}-terpinene$ were higher in mixed leaves and stems than in flowers, whereas ${\rho}cymene$ was predominantly higher in flowers than in leaves and stems.

• Horticultural Science & Technology
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• v.34 no.2
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• pp.331-341
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• 2016

We analyzed the functional fragrant components of three species of Cymbidium oriental orchids using gas chromatography-mass spectrometry (GC/MS). For the comparative analysis, C. goeringii 'Minchunran', 'Jugeumhwa', C. forrestii 'Chwigae', 'Songmae', 'Yongja', and C. faberi 'Choemae', 'Namyangmae', 'Hwaja' were investigated. Major fragrant components detected by GC/MS were selected on the basis of more than 3% value according to the analysis of peak area (%). We found that ${\alpha}$-bergamotene, which has a cytotoxic effect on breast cancer, cervical cancer, and glioblastoma, and nerolidol, which induces apoptosis of human hepatoma cells (HepG2), inhibits the growth of Streptococcus mutans and babesiosis, and has antibacterial properties, are common substances produced by C. goeringii L. Nerolidol and ${\beta}$-bisabolene, which is cytotoxic and suppresses the growth of malignant melanoma cells (B16-F10), HepG2, and leukemia cells (HL-60, K562), are major substances in C. forrestii R. Furthermore, ${\alpha}$-pinene, which inhibits the growth of gliobastoma cells (SF-767) and inhibits the anti-inflammatory action of hepatoma cells (BEL-7402); 1,8-cineole, which is a potential therapeutic agent for the treatment of gastric ulcers; and 1,3,7-octatriene, which functions as a pheromone, are the most common substances in C. faveri R. Thus, substances identified as major fragrant components in oriental orchid species have multiple beneficial applications in human health. This research forms the basis for further studies of the roles of major fragrant components in oriental orchids.

• Korean Journal of Food Science and Technology
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• v.39 no.2
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• pp.109-113
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• 2007

Adenophora remotiflora (Mosidae) is a perennial plant in the Campanulaceae family and a wild plant that only inhabits in Korea. This research analyzed the volatile compounds in Mosidae and their antioxidant activities. The volatile compounds in fresh, shady air-dried, and freeze-dried Mosidae were isolated by steam-distillation extraction (SDE) method using diethylether as a solvent. Volatile compounds were analyzed by gas chromatography-mass spectrometry (GC/MS). Antioxidant activities were determined using the linoleic acid system and 1,1-diphenyl-2-picrylhydrazyl (DPPH) method. Sixty and seventy-two volatile compounds were identified from fresh and shady air-dried Mosidae, respectively. In fresh Mosidae, the most abundant compounds were ethyl acetate and heptyl acetate, while ethyl acetate and limonene were the most abundant in the shady air-dried sample. Inhibition of peroxide formation by fresh Mosidae was higher than that of ${\alpha}-tocopherol$, and inhibition by shady air-dried Mosidae was same as that of ${\alpha}-tocopherol$. Furthermore, volatile compounds from shady air-dried Mosidae had higher free radical scavenging activity than ${\alpha}-tocopherol$. The freeze-dried sample showed lower antioxidant activity in both the linoleic acid system and DPPH method.

• Mass Spectrometry Letters
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• v.8 no.4
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• pp.114-118
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• 2017

While saliva can be considered as good biological fluid for monitoring biomarkers due to many advantages including its communication with blood and the non-invasive nature during its sampling, its applications to that purpose is still limited. As a part of efforts to expand the applications of saliva to the protein biomarker research, we carried out global absolute quantitation of proteins in human whole saliva (WS) by bottom-up proteomics techniques mainly based on nLC-Q-IMS-TOF employing $MS^E$. From the analyses of a pooled WS sample collected from 22 healthy Korean volunteers, 93 proteins ranging from $5.89{\times}10^1ng/mL$ (immunoglobulin heavy chain) to $1.59{\times}10^4ng/mL$ (${\alpha}-amylase$ 1) were confirmed. For the validation of the present results, human serum albumin in the same sample was quantitated by ELISA and its result was compared with that from the nLC-Q-IMS-TOF study. As a result, there was no significant difference between two results from individual approaches ($1.18{\times}10^4{\pm}0.03{\times}10^4 ng/mL$ from nLC-Q-IMS-TOF experiments vs. $1.23{\times}10^4{\pm}0.07{\times}10^4ng/mL$ from ELISA experiments, n=3, p=0.309). To our knowledge, this is the first global absolute quantitation of proteins in human whole saliva and information from the present study can be widely used as the first level reference for the discovery of new protein biomarkers from human whole saliva as well as for quantitative applications of human whole saliva proteins.

• BMB Reports
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• v.39 no.1
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• pp.46-54
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• 2006

The coenzyme A-acylating 2-oxoacid:ferredoxin oxidoreductase and ferredoxin (an effective electron acceptor) were purified from the hyperthermophilic archaeon, Sulfolobus solfataricus P1 (DSM1616). The purified ferredoxin is a monomeric protein with an apparent molecular mass of approximately 11 kDa by SDS-PAGE and of $11,180{\pm}50$ Da by MALDI-TOF mass spectrometry. Ferredoxin was identified to be a dicluster, [3Fe-4S][4Fe-4S], type ferredoxin by spectrophotometric and EPR studies, and appeared to be zinc-containing based on the shared homology of its N-terminal sequence with those of known zinc-containing ferredoxins. On the other hand, the purified 2-oxoacid: ferredoxin oxidoreductase was found to be a heterodimeric enzyme consisting of 69 kDa $\alpha$ and 34 kDa $\beta$ subunits by SDS-PAGE and MALDI-TOF mass spectrometry. The purified enzyme showed a specific activity of 52.6 units/mg for the reduction of cytochrome c with 2-oxoglutarate as substrate at $55^{\circ}C$, pH 7.0. Maximum activity was observed at $70^{\circ}C$ and the optimum pH for enzymatic activity was 7.0 -8.0. The enzyme displays broad substrate specificity toward 2-oxoacids, such as pyruvate, 2-oxobutyrate, and 2-oxoglutarate. Among the 2-oxoacids tested (pyruvate, 2-oxobutyrate, and 2-oxoglutarate), 2-oxoglutarate was found to be the best substrate with $K_m$ and $k_{cat}$ values of $163\;{\mu}M$ and $452\;min^{-1}$, respectively. These results provide useful information for structural studies on these two proteins and for studies on the mechanism of electron transfer between the two.

• Journal of Food Hygiene and Safety
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• v.9 no.1
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• pp.1-13
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• 1994

A Simultaneous determination method was improved for the determination and confirmation of zeranol, zearalenone, as well as their isomers and metabolites, in beef. The analytes were extracted from tissue by CH3CN, hydrolyzed enzymatically(for glucuronide conjugates), cleaned up by a strong basic anion exchange resin combined with a liquid/liquid partitioning, derivatized using MSTFA and confirmed, quantified by GC/MS/SIM with a internal standard, zearalane. The results were as follows : (1) all the estrogens were separated on the GC/MS chromatogram under the extraction method and the chromatographic conditions improved, the retention times of zearalane-TMS2, zearalanone-TMS2, zearalenone-TMS2, zeranol-TMS3, taleranol-TMS3, and $\alpha$-zearalenol-TMS3, $\beta$-zearalenol-TMS3, were 18.49, 19.44, 19.63, 19.71, 19.79 and 19.99, 20.08 minutes, respectively. (2) The calibration curves of residual zeranol, zearalenone and their metabolites showed constantly linear(r=0.99) in the range of 5~20 ng. The minimum detection concentration of residual zeranol, zearalenone and their metabolites was 1 ppb. (3) The total average recovery of residual zeranol, zearalenone and their metabolites from spiked beef was 60.2%(CV=29.7%) at the 1 ppb and 63.5%(CV=26.5) at the 2 ppb, 72.9%(CV=18.2%) at the 4 ppb. (4) The preservation method for 6 estrogens was improved for the fast running time(21 min) and MSTFA was utilized for derivatizing 6 estrogens for improvement of recovery, for good resolution, for characteristic mass spectra unlike Jose's method and Tina's method. The utilization of zearalane as internal standard showed good quantification result for zeranol, zearalenone, as well as their isomers and metabolites, in beef.

• Mass Spectrometry Letters
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• v.4 no.2
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• pp.30-33
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• 2013

Chalcones are naturally occurring, biologically active molecules generating interest from a wide range of research applications including synthetic methodology development, biological activity investigation and studying fragmentation patterns. In this article, a series of chalcones has been synthesized and their fragmentation behavior was studied using modern ambient ionization technique Direct Analysis in Real Time (DART). DART ion source connected with an ion trap mass spectrometer was used for the fragmentation of various substituted chalcones. The chalcones were introduced to the DART source using a glass capillary without sample preparation step. All the chalcones showed prominent molecular ion peaks $[M]^{{\cdot}+}$ corresponding to the structures. Multistage mass spectral data $MS^n$ ($MS^2$ and $MS^3$) were collected for all the chalcones studied. The chalcones with substitutions at 3, 4 or 5 positions gave product ion peaks with the loss of a phenyl radical ($Ph^{\cdot}$) by radical initiated ${\alpha}$-cleavage, while substitution at 2 position of chalcone in the A-ring gave a product ion peak with the loss of substituted styryl radical (PhCH = $CH^{\cdot}$). In case of the chalcones with the substituent at 4 positions in A and B rings gave both types of fragmentation patterns. In conclusion, chalcones can be easily characterized using modern DART interface in very short time and efficiently without any cumbersome sample pretreatment.

• Journal of Microbiology and Biotechnology
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• v.19 no.11
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• pp.1393-1400
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• 2009

A bacteriocin-producing strain PI80 was isolated from the gut of Penaeus indicus (Indian white shrimp) and identified as Streptococcus phocae PI80. The bacteriocin was purified from a culture supernatant to homogeneity as confirmed by Tricine SDS-PAGE. Reverse-phase HPLC analysis revealed a single active fraction eluted at 12.94 min, and MALDI-TOF mass spectrometry analysis showed the molecular mass to be 9.244 kDa. This molecular mass does not correspond to previously described streptococcal bacteriocins. The purified bacteriocin was named phocaecin PI80 from its producer strain, as this is the first report of bacteriocin production by Streptococcus phocae. The bacteriocin exhibited a broad spectrum of activity and inhibited important pathogens: Listeria monocytogenes, Vibrio parahaemolyticus, and V. fischeri. The antibacterial substance was also sensitive to proteolytic enzymes: trypsin, protease, pepsin, and chymotrypsin, yet insensitive to catalase, peroxidase, and diastase, confirming that the inhibition was due to a proteinaceous molecule (i.e., the bacteriocin), and not due to hydrogen peroxide or diacetyl. Phocaecin PI80 moderately tolerated heat treatment (up to $70^{\circ}C$ for 10 min) and resisted certain solvents (acetone, ethanol, and butanol). A massive leakage of $K^+$ ions from E. coli $DH5\alpha$, L. monocytogenes, and V. parahaemolyticus was induced by phocaecin PI80, as measured by Inductively Coupled Plasma Optical Emission Spectrometry (ICPOES). Therefore, the results of this study show that phocaecin PI80 may be a useful tool for inhibiting L. monocytogenes in seafood products that do not usually undergo adequate heat treatment, whereas the cells of Streptococcus phocae PI80 could be used to control vibriosis in shrimp farming.

• Mass Spectrometry Letters
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• v.5 no.3
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• pp.63-69
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• 2014

In this study, we present a new isotope-coded carbamidomethylation (iCCM)-based quantitative proteomics, as a complementary strategy for conventional isotope labeling strategies, with providing the simplicity, ease of use, and robustness. In iCCM-based quantification, two proteome samples can be separately isotope-labeled by means of covalently reaction of all cysteinyl residues in proteins with iodoacetamide (IAA) and its isotope (IAA-$^{13}C_2$, $D_2$), denoted as CM and iCCM, respectively, leading to a mass shift of all cysteinyl residues to be + 4 Da. To evaluate iCCM-based isotope labeling in proteomic quantification, 6 protein standards (i.e., bovine serum albumin, serotransferrin, lysozyme, beta-lactoglobulin, beta-galactosidase, and alpha-lactalbumin) isotopically labeled with IAA and its isotope, mixed equally, and followed by proteolytic digestion. The resulting CM-/iCCM-labeled peptide mixtures were analyzed using a nLC-ESI-FT orbitrap-MS/MS. From our experimental results, we found that the efficiency of iCCM-based quantification is more superior to that of mTRAQ, as a conventional nonisobaric labeling method, in which both of a number of identified peptides from 6 protein standards and the less quantitative variations in the relative abundance ratios of heavy-/light-labeled corresponding peptide pairs. Finally, we applied the developed iCCM-based quantitative method to lung cancer serum proteome in order to evaluate the potential in biomarker discovery study.