• Title/Summary/Keyword: 크로마토그래피

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Determination of cyromazine residues in agricultural commodities using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 농산물 중 Cyromazine의 잔류분석법)

  • Song, Lee-Seul;Kim, Young-Hak;Lee, Su-Jin;Hwang, Young-Sun;Kwon, Chan-Hyeok;Do, Jung-Ah;Oh, Jae-Ho;Im, Moo-Hyeog;Chang, Woo-Suk;Lee, Young-Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.16 no.3
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    • pp.202-208
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    • 2012
  • A high-performance liquid chromatographic (HPLC) method was developed to determine residues of cyromazine, a triazine insecticide, in agricultural commodities. Cyromazine was extracted with 90% aqueous methanol from representative crops which comprised brown rice, oyster mushroom, oriental melon, watermelon, and Chinese cabbage. Following to evaporation of methanol in the extract, the aqueous concentrate was acidified to form the protonated cyromazine. Dichloromethane partition was then applied to remove nonpolar co-extractives in the aqueous phase. Strong cation-exchange chromatography using Dowex 50W-X4 resin was employed for final purification of the extract. Cyromazine was successfully separated on a Zorbax SB-Aq $C_{18}$ column showing high retention for polar compounds. Cyromazine was sensitively quantitated by ultraviolet absorption at 214 nm. Limit of quantitation (LOQ) of the method was 0.04 mg/kg irrespective of sample types. Each crops were fortified at 3 different concentrations of cyromazine for recovery test. Mean recoveries from samples fortified at LOQ~2.0 mg/kg in triplicate ranged 80.2~103.3% in five agricultural commodities. Relative standard deviations in recoveries were all less than 6%. A selected-ion monitoring LC/MS method with electrospray ionization in positive-ion mode was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to routinely determine and inspect the residue of cyromazine in agricultural commodities.

Isolation and Structure Identification of Photosensitizer from Perilla frutescens Leaves Which Induces Apoptosis in U937 (들깻잎(Perilla frutescens)으로부터 U937 세포에 apoptosis를 유도하는 광과민성 물질의 분리 및 구조동정)

  • Ha, Jun Young;Kim, Mi Kyeong;Lee, Jun Young;Choi, Eun Bi;Hong, Chang Oh;Lee, Byong Won;Bae, Chang Hwan;Kim, Keun Ki
    • Journal of Life Science
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    • v.25 no.1
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    • pp.53-61
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    • 2015
  • In this study, we tried to separate the photosensitizer that induces apoptosis of leukemia cells (U937) from perilla leaves. Perilla leaves (Perilla frutescens Britt var. japonica Hara) are a popular vegetable in Korea, being rich in vitamins (A and E), GABA, and minerals. Dried perilla leaves were extracted with methanol to separate the photosensitizer by various chromatographic techniques. The structure of the isolated compound (PL9443) was identified by 1D-NMR, 2D-NMR, and FAB-mass spectroscopy. Absorbance of the UV-Vis spectrum was highest at 410 nm and was confirmed by the 330, 410, and 668 nm. PL9443 compound was determined to be pheophorbide, an ethyl ester having a molecular weight of 620. It was identified as a derivative compound of pheophorbide structure when magnesium comes away from a porphyrin ring. Observation of morphological changes in U937 cells following cell death induced by treated PL9443 compound revealed representative phenomena of apoptosis only in light irradiation conditions (apoptotic body, vesicle formation). Results from examining the cytotoxicity of PL9443 substance against U937 cells showed that inhibition rates of the cell growth were 99.9% with the concentration of 0.32 nM PL9443. Also, the caspase-3/7 activity was 99% against U937 cells with the concentration of 0.08 nM of PL9443 substance. The result of the electrophoresis was that a DNA ladder was formed by the PL9443. The PL9443 compound is a promising lead compound as a photosensitizer for photodynamic therapy of cancer.

Lipid Components of Sea Squirt, Halocynthia roretzi, and Mideuduck, Styela clava (우렁쉥이 및 미더덕의 지방질성분)

  • Lee, Eung-Ho;Oh, Kwang-Soo;Lee, Tae-Hun;Ahn, Chang-Bum;Chung, Young-Hun;Kim, Kyung-Sam
    • Korean Journal of Food Science and Technology
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    • v.17 no.4
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    • pp.289-294
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    • 1985
  • Total lipid (TL) content of sea squirt (Ureungsweng-ee), Halocynthia roretzi, and Mideuduck, Styela clava, were 2.0%, 2.1%, respectively. Reviewing the composition of each lipid fraction in total lipids of sea squirt and Mideuduck, it was found that contents of neutral lipids (NL) (36.6%, 36.3%) and phospholipids (PL) (46.2%, 44.5%) were high, while that of glycolipids (GL) (17.2%, 19.2%) was low. The NL of sea squirt and Mideuduck were mainly consisted of triglyceride (49.0%, 59.6%) and free sterol (25.8%, 22.0%), and followed by diglyceride (9.4%, 7.7%), monoglyceride (6.0%, 4.2%), free fatty acid (4.6%, 1.9%) and esterified sterol and hydrocarbon (5.2%, 4.4%). And main lipids in PL were phosphatidylcholine (48.6%, 46.7%) and phosphatidylethanolamine (32.4%, 35.0%), and followed by phosphatidylinositol (9.8%, 7.0%), phosphatidylserine (5.7%, 5.8%) and an unknown substance (3.5%, 5.5%). Fatty acid composition was not significantly different among TL, NL, PL and GL contained in sea squirt and Mideuduck. The major fatty acids of TL in sea squirt and Mideuduck were eicosapentaenoic (21.3%, 18.3%), docosahexaenoic (16.3%, 14.2%), palmitic (13.8, 16.3%) and oleic acid (8.5%, 7.0%), respectively. Fatty acid composition of PL and NL were similar to those of TL. In case of GL fraction the major fatty acids were gadoleic (15.7%, 14.7%), palmitic (13.5%, 14.7%), stearic (11.6%. 9.8%) and oleic acid (8.0%, 8.1%).

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Analysis and risk assessment of polycyclic aromatic hydrocarbons (PAHs) in seafood from oil contaminated bay (유류 오염지역의 수산물 중 다환방향족탄화수소류 (PAHs) 분석 및 위해평가)

  • Jeong, Ji-Yoon;Choi, Chan-Woong;Ryeom, Tai-Kyung;Cho, Kyoung-Hee;Park, Se-Ryung;Shin, Ho-Sang;Lee, Kwang-Ho;Lee, Hyo-Min
    • Analytical Science and Technology
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    • v.23 no.2
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    • pp.187-195
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    • 2010
  • To assess health risk for the intake among residents after the Hebei Spirit oil spill, 16 Polycyclic Aromatic Hydrocarbons (PAHs) in seafood samples from oil contaminated bay were determined by Gas Chromatography-Mass Spectrometry (GC-MSD) and samples were personally collected and purchased by residents. Samples were hydrolyzed with KOH and extracted with methylene chloride. The extracted solution were cleaned up using silica/florisil column and 16 PAHs were eluted by methylene chloride : n-hexane (1:9) mixture and determined by GC-MSD in Selected Ion Monitoring (SIM) mode. The mean recoveries for 16 PAHs ranged from 79% to 85%. The 16 PAHs levels in 126 samples ranged from 0.17 to $6.04\;{\mu}g$/kg and the TEQBaP (Toxic EQuivalents) levels in 126 samples were calculated using benzo(a)pyrene toxic equivalency factor for individual 16 PAHs and ranged from 0 to $0.91\;{\mu}gTEQ$/kg. The average Benzo(a)pyrene dietary exposure of residents was $5.5{\times}10^{-8}\;mg/kg$ bw/day and the average PAHs chronic dietary exposure was $1.3{\times}10^{-5}\;mg$ TEQ/kg bw/day. The margin of exposure (MOE) and the excess cancer risk and were $1.8{\times}10^6$ and $9.8{\times}10^{-8}$, respectively. Therefore, the assessment result was considered as low concern for health risk.

Risk Analysis of Inorganic Arsenic in Foods (식품 중 무기비소의 위해 분석)

  • Yang, Seung-Hyun;Park, Ji-Su;Cho, Min-Ja;Choi, Hoon
    • Journal of Food Hygiene and Safety
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    • v.31 no.4
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    • pp.227-249
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    • 2016
  • Arsenic and its compounds vary in their toxicity according to the chemical forms. Inorganic arsenic is more toxic and known as carcinogen. The provisional tolerable weekly intake (PTWI) of $15{\mu}g/kg$ b.w./week established by the Joint FAO/WHO Expert Committee on Food Additives (JECFA) has been withdrawn, while the EFSA panel suggested $BMDL_{0.1}$ $0.3{\sim}8{\mu}g/kg\;b.w./day$ for cancers of the lung, skin and bladder, as well as skin lesions. Rice, seaweed and beverages are known as food being rich in inorganic arsenic. As(III) is the major form of inorganic arsenic in rice and anaerobic paddy soils, while most of inorganic arsenic in seaweed is present as As(V). The inorganic arsenic in food was extracted with solvent such as distilled water, methanol, nitric acid and so on in heat-assisted condition or at room temperature. Arsenic speciation analysis was based on ion-exchange chromatography and high-performance liquid chromatography equipped with atomic absorption spectrometry and inductively coupled plasma mass spectrometry. However, there has been no harmonized and standardized method for inorganic arsenic analysis internationally. The inorganic arsenic exposure from food has been estimated to range of $0.13{\sim}0.7{\mu}g/kg$ bw/day for European, American and Australian, and $0.22{\sim}5{\mu}g/kg$ bw/day for Asian. The maximum level (ML) for inorganic arsenic in food has established by EU, China, Australia and New Zealand, but are under review in Korea. Until now, several studies have conducted for reduction of inorganic arsenic in food. Inorganic arsenic levels in rice and seaweed were reduced by more polishing and washing, boiling and washing, respectively. Further research for international harmonization of analytical method, monitoring and risk assessment will be needed to strengthen safety management of inorganic arsenic of foods in Korea.

Characterization of Bacteriocin Produced from Isolated Strain of Bacillus sp. (Bacillus 속 분리주가 생산하는 박테리오신의 특성 조사)

  • Ham, Seung-Hee;Choi, Nack-Shick;Moon, Ja-Young;Baek, Sun-Hwa;Lee, Song-Min;Kang, Dae-Ook
    • Journal of Life Science
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    • v.27 no.2
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    • pp.202-210
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    • 2017
  • As an effort to find a potential biopreservative, we isolated bacterial strains producing bacteriocin from fermented foods. A strain was finally selected and characteristics of the bacteriocin were investigated. The selected strain was identified as Bacillus subtilis E9-1 based on the 16S rRNA gene analysis. The culture supernatant of B. subtilis E9-1 showed antimicrobial activity against Gram-positive bacteria. Subtilisin A, ${\alpha}$-chymotrypsin, trypsin and proteinase K inactivated the antimicrobial activity, which means its proteinaceous nature, a bacteriocin. The bacteriocin activity was fully retained at the pH range from 2.0 to 8.0 and stable at up to $100^{\circ}C$ for 60 min. Solvents such as ethanol, isopropanol and methanol had no effect on the antimicrobial activity at the concentration of 100% but acetone and acetonitrile reduced the activity at up to 100% concentration. Cell growth of four indicator strains was dramatically decreased in dose-dependent manner. Listeria monocytogenes was the most sensitive, but Enterococcus faecium was the most resistant. Bacillus cereus and Staphylococcus aureus showed the medium sensitivity. The bacteriocin showed its antimicrobial activity against B. cereus and L. monocytogenes via bactericidal action. The number of viable cells of L. monocytogenes started to reduce after addition of bacteriocin to the minced beef. The bacteriocin was purified through acetone concentration, gel filtration chromatography and RP-HPLC. The whole purification step led to a 6.82 fold increase in the specific activity and 6% yield of bacteriocin activity. The molecular weight of the purified bacteriocin was determined to be 3.3 kDa by MALDI-TOF/TOF mass spectrometry.

A Study on the Pollution of Polycyclic Aromatic Hydrocarbons(PAHs) in the Surface Sediments Around Gwangyang Bay (광양만 주변해역 표층퇴적물에서의 다환방향족탄화수소류(PAHs)의 오염에 관한 연구)

  • You, Young-Seok;Choi, Young-Chan;Cho, Hyeon-Seo
    • Journal of the Korean Society of Marine Environment & Safety
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    • v.13 no.1 s.28
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    • pp.9-20
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    • 2007
  • PAHs(Polycyclic Aromatic Hydrocarbons) are widespread contaminants in the marine environment. They are of mainly anthropogenic origin from urban runoff, oil spill and combustion of fossil fuels. Some PAHs are potentially carcinogenic and mutagenic to aquatic organism The contamination of PAHs in the coastal environments has not been well known yet in Korea. This study was carried out to survey the contamination of PAHs in sediments around Gwangyang bay. The Yeosu petrochemical industrial complex, POSCO(Pohang steel company) and Gwangyang container harbor are located around the bay. PAHs in sediment samples were extracted in soxhlet extractor and were identified and quantified by GC-MS(Gas Chromatography-Mass Spectrometry) TOC(Total Organic carbon) and textural parameters in sediment samples were also analyzed 13 species of PAHs were detected at all of the surface sediments. Total PAHs concentrations in the surface sediments ranged from 171.40 to $1013.54{\mu}g/kg$ dry wt.. In most of the surface sediments, Naphthalene was the highest in the range of 14.08 to $691.39{\mu}g/kg$ dry wt. and Anthracene was the lowest in the range of 0.49 to $22.66{\mu}g/kg$ dry wt.. The correlation coefficients between individual PAHs and Total PAHs in the surface sediments were relatively higher in the low molecular compounds such as Naphthalene and Phenanthrene. In the relationship of the P/A(Phenanthrene/Anthracene) ratio and F/P(Fluoranthene/Pyrene) ratio, P/A ratio was generally above 10 and F/P ratio was shown to be above 1 in all sediment samples. These data indicate that PAHs in sediments around Gwangyang bay seem to be of both pyrolytic and petrogenic origin. Total PAHs in the surface sediments were correlated with TOC and textural parameters. The values of PAHs in the surface and core sediments were lower than the biological effect guidelines.

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Antioxidative Effect and Neuraminidase Inhibitory Activity of Polyphenols Isolated from a New Korean Red Waxy Sorghum (Sorghum bicolor L. cv. Hwanggeumchalsusu) (황금찰수수(Sorghum bicolor L. cv. Hwanggeumchalsusu) 유래 에탄올 추출물 및 폴리페놀계 화합물의 항산화 활성 및 뉴라미니데이즈 억제 효과)

  • Ra, Ji-Eun;Seo, Kyung Hye;Ko, Jee Yeon;Lee, Mi-Ja;Kang, Hyeon Jung;Kim, Sun Lim;Chung, Ill-Min;Seo, Woo Duck
    • Journal of Life Science
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    • v.25 no.7
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    • pp.786-794
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    • 2015
  • To identify nutritional and therapeutic properties of the new Korean red waxy sorghum cultivar ‘Hwanggeumchalsusu (HGC)’, we assayed the antioxidative effects and neuraminidase inhibitory activity. A methanol and 70% ethanol extract of HGC exhibited strong antioxidative effects (IC50 values of 83.2±2.7 for DPPH) and 85.6±2.4 μg/ml for ABTS) and neuraminidase (ND) inhibitory activity (IC50 values of 1.8±0.1 from extracted with methanol and 3.4±0.1 μg/ml from extracted with 70% ethanol) compared with that of the control, noncolored sorghum cultivar ‘Huinchalsusu (HC)’ (IC50> 200 μg/ml). We isolated nine polyphenols, Gallic acid (1), Protocatecuic acid (2), p-Hydroxy benzoic acid (3), Vanillic acid (4), Caffeic acid (5), Ferulic acid (6), Luteolinidin (7), Apigeninidin (8), Luteolin (9), from the HGC - methanol extract, to determine whether they were the active components Luteolinidin of one kind of polyphenols from the HGC, exhibited significant antioxidative effects (IC50 values of 10.9±0.5 μM for DPPH and 8.6 0.6 μM for ABTS) and neuraminidase (ND) inhibitory activity (IC50 values of 26.3±0.6) showed noncompetitive inhibition model. The binding affinity of the ND inhibitors in molecular docking experiments correlated with their ND inhibitory activities. These results suggest that HGC may be utilized to serve as a potential effective antioxidant and inhibitor of ND.

Isolation and Identification of a Photosensitizer from Pueraria thunbergiana Leaves that Induces Apoptosis in SK-HEP-1 Cells (P. thunbergiana 잎으로부터 SK-HEP-1세포에 대한 apoptosis를 유도하는 광과민성물질의 분리 및 구조동정)

  • Lee, Jun Young;Kim, Mi Kyeong;Ha, Jun Young;Kim, Yong Gyun;Hong, Chang Oh;Kim, So Young;Kim, Chung-Hwan;Kim, Keun Ki
    • Journal of Life Science
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    • v.24 no.3
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    • pp.242-251
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    • 2014
  • The objective of this study was to isolate a photosensitizer from Pueraria thunbergiana leaves that induces apoptosis in SK-HEP-1 cells. Column chromatography and thin layer chromatography were used to isolate active compounds from extracts of P. thunbergiana leaves. The structures of the isolated compounds were determined by 1D-NMR, 2D-NMR, and FAB-mass spectroscopy. A substance, named M4-3, was purified from the leaves of P. thunbergiana using various chromatography methods, and the absorbance of the substance was measured. The absorbance was highest at 410 nm, suggesting that the M4-3 substance was a different compound from chlorophyll a and b, which absorb at 410, 502, 533, and 607 nm. Further analyses revealed that the M4-3 compound was a $13^2$-hydoxy pheophorbide, a methyl ester with a molecular weight of 662. M4-3 was identified as a derivative compound of pheophorbide, with a structure that magnesium comes away from the porphyrin ring. The results of the analysis of the cytotoxicity of the M4-3 substance against the SK-HEP-1 cells revealed that it inhibited rates of cell growth by 40% and 80% at a concentration of 0.04 ${\mu}M$ and 0.08 ${\mu}M$, respectively. The M4-3 compound was found to be a photosensitizer for cytotoxicity because it was appeared only in light condition as examining activity in different irradiation conditions (light condition and nonlight condition) under the same concentration. Analysis of morphological changes in the cells following cell death induced by exposure to the M4-3 substance reveled representative phenomena of apoptosis (nuclear condensation, vesicle formation, and fragmentation of DNA). The induction of apoptosis was attributed to the compound's photodynamic activity.

Evaluation of Basin-Specific CH4 emission flux from Intertidal Flat Sediments of Sogeun-ri, Taean, Mid-west Korea (한국 서해안 태안 소근리 갯벌의 메탄가스 발생량 특성)

  • Lee, Jun-Ho;Jeong, Kap-Sik;Woo, Han Jun;Kang, Jeongwon;Lee, Dong-Hun;Jang, Seok;Kim, Seong-Ryul
    • Journal of Wetlands Research
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    • v.16 no.2
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    • pp.281-291
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    • 2014
  • In March to August 2013, the emission of gases ($CH_4$, VOC, $CO_2$, $O_2$, and LEL) was measured three times from the intertidal flat sediments at Sogeun-ri, Taean-gun, in the Mid-western seashore of Korea by using chamber method. After analyzing gas emission concentrations inside of flux enclosure chamber by using a GC equipped with Agilent 6890. The gas emission fluxes were calculated from a linear regression of the changes in the concentrations with time. The ranges of gas flux during the experimental period were $+0.06{\sim}+0.60mg/m^2/hr$ for $CH_4$, $+58.45{\sim}+95.58mg/m^2/hr$ for $CO_2$, $-0.02{\sim}-0.20mg/m^2/hr$ for $O_2$, and $-0.60{\sim}+0.65mg/m^2/hr$ for VOC, respectively. The flux measurement results revealed that $CH_4$ fluxes during March in the relatively low sediment temperature ($14.5^{\circ}C$) were significantly higher ($+0.60mg/m^2/hr$) than during June and August ($+0.06{\sim}+0.18mg/m^2/hr$) in high sediment temperature ($32.0{\sim}36.8^{\circ}C$). $CH_4$ flux to mean size of sediments and temperature of inner chamber exhibited strong positive correlation ($R^2=-0.97$ and $R^2=-0.89$, respectively).