• Title/Summary/Keyword: GC/M S-SIM

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Development of the analytical method for pesticide residues in crops by using gas chromatograph / solvent free solid injector (GC / SFSI) (무용매 고체 시료 주입기(SFSI)를 이용한 작물 중 잔류농약의 기체크로마토그래피 분석법 개발)

  • Kim, M.R.;Lee, Y.;Park, B.J.;Choi, J.H.;Kim, I.S.;Shim, J.H.
    • The Korean Journal of Pesticide Science
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    • v.9 no.3
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    • pp.237-242
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    • 2005
  • This experiment was carried out to develop the fast and simple method for pesticide residue analysis by using solvent free solid injector (SFSI) and to validate the efficiency of the method developed for the residue analysis of the endocrine disruptor-like pesticides such as endosulfan, metribuzin, trifluralin and vinclozolin. The samples after freeze drying were sealed in glass capillary tubes and then introduced into the heated injector of gas chromatogaphy. The required pre-heating times were 1 min for endosulfan and trifluralin, 5 min for vinclozolin, and 10 min for metribuzin. The detection limits of endosulfan in chinese cabbages, metribuzin in lettuces, trifluralin in spinachs and vinclozolin in hot peppers were 0.05, 0.1, 0.05 and 0.05 ng, respectively and their recoveries were ranged from 74%, $98{\sim}107%$, $86{\sim}95%$ and $94{\sim}95%$, respectively. The detected level of metribuzine residue in field lettuce samples by using the SFSI was 0.6 ng/mg.

Brief Introduction of Research Progresses in Control and Biocontrol of Clubroot Disease in China

  • He, Yueqiu;Wu, Yixin;He, Pengfei;Li, Xinyu
    • 한국균학회소식:학술대회논문집
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    • 2015.05a
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    • pp.45-46
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    • 2015
  • Clubroot disease of crucifers has occurred since 1957. It has spread to the whole China, especially in the southwest and nourtheast where it causes 30-80% loss in some fields. The disease has being expanded in the recent years as seeds are imported and the floating seedling system practices. For its effective control, the Ministry of Agriculture of China set up a program in 2010 and a research team led by Dr. Yueqiu HE, Yunnan Agricultural University. The team includes 20 main reseachers of 11 universities and 5 institutions. After 5 years, the team has made a lot of progresses in disease occurrence regulation, resources collection, resistance identification and breeding, biological agent exploration, formulation, chemicals evaluation, and control strategy. About 1200 collections of local and commercial crucifers were identified in the field and by artificiall inoculation in the laboratories, 10 resistant cultivars were breeded including 7 Chinese cabbages and 3 cabbages. More than 800 antagostic strains were isolated including bacteria, stretomyces and fungi. Around 100 chemicals were evaluated in the field and greenhouse based on its control effect, among them, 6 showed high control effect, especially fluazinam and cyazofamid could control about 80% the disease. However, fluzinam has negative effect on soil microbes. Clubroot disease could not be controlled by bioagents and chemicals once when the pathogen Plasmodiophora brassicae infected its hosts and set up the parasitic relationship. We found the earlier the pathogent infected its host, the severer the disease was. Therefore, early control was the most effective. For Chinese cabbage, all controlling measures should be taken in the early 30 days because the new infection could not cause severe symptom after 30 days of seeding. For example, a biocontrol agent, Bacillus subtilis Strain XF-1 could control the disease 70%-85% averagely when it mixed with seedling substrate and was drenching 3 times after transplanting, i.e. immediately, 7 days, 14 days. XF-1 has been deeply researched in control mechanisms, its genome, and development and application of biocontrol formulate. It could produce antagonistic protein, enzyme, antibiotics and IAA, which promoted rhizogenesis and growth. Its The genome was sequenced by Illumina/Solexa Genome Analyzer to assembled into 20 scaffolds then the gaps between scaffolds were filled by long fragment PCR amplification to obtain complet genmone with 4,061,186 bp in size. The whole genome was found to have 43.8% GC, 108 tandem repeats with an average of 2.65 copies and 84 transposons. The CDSs were predicted as 3,853 in which 112 CDSs were predicted to secondary metabolite biosynthesis, transport and catabolism. Among those, five NRPS/PKS giant gene clusters being responsible for the biosynthesis of polyketide (pksABCDEFHJLMNRS in size 72.9 kb), surfactin(srfABCD, 26.148 kb, bacilysin(bacABCDE 5.903 kb), bacillibactin(dhbABCEF, 11.774 kb) and fengycin(ppsABCDE, 37.799 kb) have high homolgous to fuction confirmed biosynthesis gene in other strain. Moreover, there are many of key regulatory genes for secondary metabolites from XF-1, such as comABPQKX Z, degQ, sfp, yczE, degU, ycxABCD and ywfG. were also predicted. Therefore, XF-1 has potential of biosynthesis for secondary metabolites surfactin, fengycin, bacillibactin, bacilysin and Bacillaene. Thirty two compounds were detected from cell extracts of XF-1 by MALDI-TOF-MS, including one Macrolactin (m/z 441.06), two fusaricidin (m/z 850.493 and 968.515), one circulocin (m/z 852.509), nine surfactin (m/z 1044.656~1102.652), five iturin (m/z 1096.631~1150.57) and forty fengycin (m/z 1449.79~1543.805). The top three compositions types (contening 56.67% of total extract) are surfactin, iturin and fengycin, in which the most abundant is the surfactin type composition 30.37% of total extract and in second place is the fengycin with 23.28% content with rich diversity of chemical structure, and the smallest one is the iturin with 3.02% content. Moreover, the same main compositions were detected in Bacillus sp.355 which is also a good effects biocontol bacterial for controlling the clubroot of crucifer. Wherefore those compounds surfactin, iturin and fengycin maybe the main active compositions of XF-1 against P. brassicae. Twenty one fengycin type compounds were evaluate by LC-ESI-MS/MS with antifungal activities, including fengycin A $C_{16{\sim}C19}$, fengycin B $C_{14{\sim}C17}$, fengycin C $C_{15{\sim}C18}$, fengycin D $C_{15{\sim}C18}$ and fengycin S $C_{15{\sim}C18}$. Furthermore, one novel compound was identified as Dehydroxyfengycin $C_{17}$ according its MS, 1D and 2D NMR spectral data, which molecular weight is 1488.8480 Da and formula $C_{75}H_{116}N_{12}O_{19}$. The fengycin type compounds (FTCPs $250{\mu}g/mL$) were used to treat the resting spores of P. brassicae ($10^7/mL$) by detecting leakage of the cytoplasm components and cell destruction. After 12 h treatment, the absorbencies at 260 nm (A260) and at 280 nm (A280) increased gradually to approaching the maximum of absorbance, accompanying the collapse of P. brassicae resting spores, and nearly no complete cells were observed at 24 h treatment. The results suggested that the cells could be lyzed by the FTCPs of XF-1, and the diversity of FTCPs was mainly attributed to a mechanism of clubroot disease biocontrol. In the five selected medium MOLP, PSA, LB, Landy and LD, the most suitable for growth of strain medium is MOLP, and the least for strains longevity is the Landy sucrose medium. However, the lipopeptide highest yield is in Landy sucrose medium. The lipopeptides in five medium were analyzed with HPLC, and the results showed that lipopeptides component were same, while their contents from B. subtilis XF-1 fermented in five medium were different. We found that it is the lipopeptides content but ingredients of XF-1 could be impacted by medium and lacking of nutrition seems promoting lipopeptides secretion from XF-1. The volatile components with inhibition fungal Cylindrocarpon spp. activity which were collect in sealed vesel were detected with metheds of HS-SPME-GC-MS in eight biocontrol Bacillus species and four positive mutant strains of XF-1 mutagenized with chemical mutagens, respectively. They have same main volatile components including pyrazine, aldehydes, oxazolidinone and sulfide which are composed of 91.62% in XF-1, in which, the most abundant is the pyrazine type composition with 47.03%, and in second place is the aldehydes with 23.84%, and the third place is oxazolidinone with 15.68%, and the smallest ones is the sulfide with 5.07%.

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Quantification of 4-Hydroxyalkenals in Oils Consumed in Korea (상용하는 식물성 기름에서 지질과산화의 독성물질 4-hydroxy-2-alkenals 정량)

  • Surh, Jeong-Hee;Kwon, Hoon-Jeong
    • Korean Journal of Food Science and Technology
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    • v.34 no.5
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    • pp.905-910
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    • 2002
  • 4-Hydroxyalkenals are cytotoxic aldehydes generated by the oxidation of n-6 and n-3 polyunsaturated fatty acids. To evaluate the potential risk of 4-hydroxyalkenals on Koreans, quantitative data of various oils are necessary. Simultaneous monitoring of 4-hydroxyhexenal and 4-hydroxynoneal in 39 samples including new and used ones through single ion monitoring mode of GC/MS detected both aldehydes in all samples tested, ranging from 0.21 to 26.9 nmol/g for 4-hydroxy-2-hexenal and 0.06 to 56.6 nmol/g for 4-hydroxy-2-nonenal. Frying oils collected from local markets showed 2.28-7.90 and 8.31-30.5 nmol/g of 4-hydroxyhexenal and 4-hydroxynoneal, respectively. National health and nutrition survey data were employed to determine the exposure effect to these 4-hydroxyalkenals from the four most consumed oils in Korea. Daily exposures to hydroxyalkenals excluding possible exposure from fried food were $1.9\;{\mu}g$ from soybean oil, $0.5\;{\mu}g$ from sesame oil, $0.2\;{\mu}g$ from corn oil, and $0.1\;{\mu}g$ from perilla oil. Due to the increasing consumption of polyunsaturated fatty acids in Korea, these data may provide valuable information for evaluating possible physiological effects of 4-hydroxyalkenals from vegetable oils.

A Study on the BTEX Ratio and Correlation of C2-benzenes in Vehicle Exhaust (자동차 배출가스 중 BTEX의 비율과 C2-benzenes의 상관성 연구)

  • Mun, Sunhee;Chung, Taekho;Jung, Sungwoon;Kim, Sunmoon;Seo, Seokjun;Lee, Seounghwan;Kim, Jounghwa;Hong, Youdeog;Hong, Heekyoung
    • Journal of ILASS-Korea
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    • v.23 no.4
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    • pp.185-191
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    • 2018
  • Benzene, toluene, ethylbenzene and xylene (BTEX) were well known as ozone precursors from photochemical reactions and contribute to the formation of photochemical smog which pose health hazards. Also, some of these compounds directly affect the human health due to their toxicity such as benzene. In this study, BTEX ratios and correlation of $C_2$-benzenes (xylenes, ethylbenzene) in vehicle exhaust from recreational vehicle (RV) and multi-purpose vehicle (MPV) were characterized using a chassis dynamometer. VOCs were collected by tedlar bag and a GC/MS system was used for their quantification. Among all of the BTEX, toluene has the highest concentration(more than 30% in composition of BTEX). The average ratio of toluene to benzene emissions (T/B ratio=2.2) was found in vehicle exhaust. The average m,p-xylene/ethylbenzene and m,p-xylene/o-xylene ratios were 1.0 and 3.0 respectively. As a result, it showed a good correlation between the $C_2$-benzenes ($R^2=0.98{\sim}0.99$). In the future, it can be used as a marker for effect evaluation to atmospheric environment by vehicle exhaust.

Physicochemical properties of deposited particles on surface of pine leaves as biomarker for air pollution (솔잎가지 표면에 침착된 입자상 물질의 물리화학적 특성 및 대기오염 지표로서의 가능성 고찰)

  • Chung, David;Choi, Jeong-Heui;Lee, Jang-Ho;Lee, Soo-Yong;Lee, Ha-Eun;Park, Ki-Wan;Shim, Kyu-Young;Lee, Jong-Chun
    • Analytical Science and Technology
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    • v.31 no.6
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    • pp.247-258
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    • 2018
  • The purpose of the present study was to investigate whether the degree of air pollution can be evaluated via examination of local plants. Selected sites included two parks in an industrial area, as well as two parks in an urban area. Selected plant samples comprised one-year-old pine shoot leaves. Leaves growing over 2 m from the ground were collected from over 10 pine trees. Leaf surface was analyzed for deposition of 14 trace elements and 16 polycyclic aromatic hydrocarbons (PAHs), including particle size and mass, surface imaging, precipitation-mediated particle removal rate, and concentration. Particle size ranged from 0.4 to $200{\mu}m$, and the volume percentage of particles ${\leq}10$ was 20 %. Deposited particle mass ranged from 0.450-0.825 mg, and precipitation-mediated removal rate ranged from 10.0-27.6 %. Trace element concentration, as measured by ICP/MS after microwave acid digestion, was 18.8-26.3 mg/kg As, 0.08-0.13 mg/kg Be, 0.06-0.08 mg/kg Cd, 4.91-17.8 mg/kg Cr, 5.26-405 mg/kg Cu, 1,930-2,670 mg/kg Fe, 3.03-28.1 mg/kg Pb, 26.9-42.8 mg/kg Mn, 2.66-10.4 mg/kg Ni, 4,560-8,730 mg/kg Al, 2,500-6,120 mg/kg Ba, 5.27-17.8 mg/kg Rb, 40.9-95.3 mg/kg Sr, and 4,030-8,260 mg/kg Zn. Concentration of PAHs, as analyzed by GC/MS/MS after liquid-liquid extraction and purification of deposited particles, ranged from 1.17 to 12.378 mg/kg for ${\Sigma}PAH_{16}$ and from 1.17 to 12.378 mg/kg for ${\Sigma}PAH_7$.

REMINERALIZATION DEPTH OF CPP-ACP ON DEMINERALIZATION HUMAN ENAMEL IN VITRO (탈회된 법랑질에서 CPP-ACP의 재광화 깊이)

  • Choi, Han-Ju;Choi, Yeong-Chul;Kim, Kwang-Chul;Choi, Sung-Chul
    • Journal of the korean academy of Pediatric Dentistry
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    • v.35 no.2
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    • pp.278-286
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    • 2008
  • Many studies regarding Casein phosphopeptides-amorphous calcium phosphate(CPP-ACP) have demonstrated the remineralization ability on the demineralized enamel surface. A question is still remained that how deep can the calcium (Ca) and phosphorus (P) ions supplied by the CPP-ACP paste penetrate into the enamel subsurface. The aims of this study were to measure the penetrating depth of Ca and P ions in the demineralized human enamel in vitro, and were to determine the amount and depth of Ca and P ions according to the duration. The amount and depth of Ca and P ions were measured by microscopic observation with Field Emission Scanning Electron Microscopy (FE-SEM; LEO SUPRA 55, Carl Zeiss, Germany) and Energy Dispersive X-ray Spectrometer (EDS; GENESIS 2000, EDAX, USA: Linescan of Calcium and Phosphorus). Freshly extracted four human 1st premolars were obtained from the Dept. of Pediatric Dent., Kyung Hee Univ. Buccal surfaces of the 1st premolars were covered with nail varnish to form a window on the middle third of buccal surface. All of the teeth with enamel windows were immersed in a solution of 0.1 M lactic acid, Carbopol C907 (carboxypolymethylene BF Goodrich, Cleveland, OH, USA) at pH 4.8, and then incubated for 7 days. Each tooth crown was sawn in half through the midline of buccal window along the long axis of premolar. The four blocks of premolars were immersed in a 10-times diluted solution of CPP-ACP paste (Tooth Mousse, GC Corp., Tokyo, Japan) for 1, 2, 3 and 5 weeks while the rests were immersed in a placebo solution (distilled water) for the same duration. Each specimen was embedded in epoxy resin, and was sectioned perpendicular to the window, using a water-cooled diamond blade saw. The spectrum density indices of Ca and P were measured in the sound, de- and remineralized enamels by FE-SEM and EDS. The Student's t test was performed to compare the Spectrum Density Indices (SDI) of sound, re-and demineralized enamels, and to compare the differences among the durations. Followings are the conclusion : 1. The penetration depth of the remineralizing ions (Ca & P) of CPP-ACP paste is related to the depth of demineralized enamel (approximately $1050{\sim}1350{\mu}m$). It is revealed that the penetration depth of both ions reaches full thickness of decalcification and even slightly into the sound enamel. 2. The Ca & P levels of remineralized enamels in 1, 2 weeks were significantly higher than those of the sound enamels (p<0.05). 3. No statistically significant difference of Ca & P levels was found in relation with the increasing duration of remineralization (p>0.05).

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CHEMICAL DEGRADATION OF LIGHT-CURED DENTAL COMPOSITE RESINS (수종 치과용 광중합형 복합레진의 화학적 분해)

  • Yang, Kuy-Ho;Choi, Nam-Ki;Park, Mi-Ran;Park, Eun-Hae
    • Journal of the korean academy of Pediatric Dentistry
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    • v.28 no.3
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    • pp.403-411
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    • 2001
  • The aim of this study was to evaluate the resistance to degradation of four commercial composite resins in an alkaline solution. The brands studied were Unifil(GC, Japan), Palfique(Tokuyama Japan). Definite$Degussa-H\ddot{u}ls$ AG, Germany). Revolution(Kerr, U.S.A.). Preweighed discs of each brand were exposed 0.1N NaOH solution at $60^{\circ}C$. After 14 days they were removed, neutralized with HCl, washed with water and dried. Resistance to degradation was evaluated on the basis of following parameters: (a) mass loss(%) - determined from pre-and post-exposed specimen weights; (b) Si loss(ppm) - obtained from ICP-AE analysis of solution exposed to specimens; and (c) degradation depth$({\mu}m)$ - measured microscopically (SEM) from polished circular sections of exposed specimens. The results were follows: 1. The mass loss of Unifil was 3.21%, it was the highest of materials. But, there was no significant difference among the materials. 2. The degree of degradation layer depth was $107.69\sim47.40{\mu}m$, the sequence of the degree pf degradation layer depth was in descending order by Unifil, Palfique, Revolution, Definite. There was significant difference among the materials except Palfique and Definite. 3. The Si loss of Paltique was 8940.0ppm, it was the highest. There was significant difference among the materials, except Revolution and Definite(p<0.05). 4. The correlation coefficient between mass loss and degradation depth was relatively high(r = 0.06, p<0.05). 5. There was no significant coefficient correlation between Si loss and mass loss, and/or the degree of degradation layer depth and Si loss. 6. When observed with SEM, destruction of bonding is observed between resin matrix and filler. Above results suggested that the hydrolytic degradation is considered as evaluation factor of composite resins.

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A Study on Detection Characteristics of Cadmium and Lead for Bi Nanopowder-Labeled Electrode (비스무스 나노분말 표지 전극의 카드뮴/납 검출특성에 관한 연구)

  • Lee, Gyeoung-Ja;Kim, Hyoun-Jin;Lee, Hi-Min;Lee, Sang-Hoon;Lee, Min-Ku;Lee, Chang-Kyu
    • Journal of Powder Materials
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    • v.15 no.5
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    • pp.393-398
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    • 2008
  • Trace analysis of Cd and Pb at surface modified thick film graphite electrode with Bi nanopowder has been carried out using square-wave anodic stripping voltammetry (SWASV) technique. Bi nanopowder synthesized by gas condensation (GC) method showed the size of $50{\sim}100$ nm with BET surface area, $A_{BET}=6.8m^{2}g^{-l}$. For a strong adhesion of the Bi nanopowder onto the screen printed carbon paste electrode, nafion solution was added into Bi-containing suspension. From the SWASV, it was found that the Bi nanopowder electrode exhibited a well-defined responses relating to the oxidations of Cd and Pb. The current peak intensity increased with increasing concentration of Cd and Pb. From the linear relationship between Cd/Pb concentrations and peak current, the sensitivity of the Bi nanopowder electrode was quantitatively estimated. The detection limit of the electrode was estimated to be $0.15{\mu}g/l$ and $0.07{\mu}g/l$ for Cd and Pb, respectively, on the basis of the signal-to-noise characteristics (S/N=3) of the response for the $1.0{\mu}g/l$ solution under a 10 min accumulation.

Salinity Stress Resistance Offered by Endophytic Fungal Interaction Between Penicillium minioluteum LHL09 and Glycine max. L

  • Khan, Abdul Latif;Hamayun, Muhammad;Ahmad, Nadeem;Hussain, Javid;Kang, Sang-Mo;Kim, Yoon-Ha;Adnan, Muhammad;Tang, Dong-Sheng;Waqas, Muhammad;Radhakrishnan, Ramalingam;Hwang, Young-Hyun;Lee, In-Jung
    • Journal of Microbiology and Biotechnology
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    • v.21 no.9
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    • pp.893-902
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    • 2011
  • Endophytic fungi are little known for their role in gibberellins (GAs) synthesis and abiotic stress resistance in crop plants. We isolated 10 endophytes from the roots of field-grown soybean and screened their culture filtrates (CF) on the GAs biosynthesis mutant rice line - Waito-C. CF bioassay showed that endophyte GMH-1B significantly promoted the growth of Waito-C compared with controls. GMH-1B was identified as Penicillium minioluteum LHL09 on the basis of ITS regions rDNA sequence homology and phylogenetic analyses. GC/MS-SIM analysis of CF of P. minioluteum revealed the presence of bioactive $GA_4$ and $GA_7$. In endophyte-soybean plant interaction, P. minioluteum association significantly promoted growth characteristics (shoot length, shoot fresh and dry biomasses, chlorophyll content, and leaf area) and nitrogen assimilation, with and without sodium chloride (NaCl)-induced salinity (70 and 140 mM) stress, as compared with control. Field-emission scanning electron microcopy showed active colonization of endophyte with host plants before and after stress treatments. In response to salinity stress, low endogenous abscisic acid and high salicylic acid accumulation in endophyte-associated plants elucidated the stress mitigation by P. minioluteum. The endophytic fungal symbiosis of P. minioluteum also increased the daidzein and genistein contents in the soybean as compared with control plants, under salt stress. Thus, P. minioluteum ameliorated the adverse effects of abiotic salinity stress and rescued soybean plant growth by influencing biosynthesis of the plant's hormones and flavonoids.

Gibberellin A7 production by Aspergillus tubingensis YH103 and cultural characteristics of endophytic fungi isolated from Tetragonia tetragonoides in Dokdo islands (독도 번행초에서 분리된 내생균류의 배양적 특성과 Aspergillus tubingensis YH103의 gibberellin A7의 생산)

  • You, Young-Hyun;Park, Jong Myong;Lim, Sung Hwan;Kang, Sang-Mo;Park, Jong-Han;Lee, In-Jung;Kim, Jong-Guk
    • Korean Journal of Microbiology
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    • v.52 no.1
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    • pp.32-39
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    • 2016
  • Coastal plant species Tetragonia tetragonoides (Pall.) Kuntze native to the Dokdo islands was sampled and then 17 endophytic fungi were purely isolated based on morphological differences. The fungal isolates were characterized by their growth properties under NaCl concentration or pH gradient. Culture filtrates of the 17 fungal isolates were treated to Waito-c rice (WR) seedlings for verifying plant growth-promoting activity. As the results, YH103 strain showed the highest plant growth-promoting activity among them. Phylogenetic analysis of the isolates was done by the maximum likelihood method based on partial internal transcribed spacer region (ITS region: contaning ITS1, 5.8S, and ITS2), beta-tubulin (BenA), and calmodulin (CaM) gene sequences. Chromatographic analysis of the strain YH103 culture filtrate showed the existence of gibberellins ($GA_4$, $GA_7$, $GA_8$, and $GA_{19}$). Finally, the strain YH103 was identified as Aspergillus tubingensis by microscopic observation and molecular analysis and, to our knowledge, this is the first report of GAs producing A. tubingensis.