• Title/Summary/Keyword: ether extraction

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Polarity affects the antioxidant and antimicrobial activities of jellyfish (Acromitus hardenbergi) extracts

  • Khong, Nicholas M.H.;Foo, Su Chern;Yau, Sook Kun;Chan, Kim Wei;Yusoff, Fatimah Md.
    • Fisheries and Aquatic Sciences
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    • v.25 no.4
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    • pp.189-201
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    • 2022
  • Jellyfish is an emerging aquaculture species, farmed for Oriental cuisines and nutraceutical ingredients. This study aimed to examine antioxidative and antimicrobial potentials of various fractions of the jellyfish, Acromitus hardenbergi. The bell and oral arms of the jellyfish were sequentially extracted with petroleum ether (PE), dichloromethane (DCM), chloroform (CHCl3), methanol (MeOH), and water (H2O) to extract its bioactive in an increasing polarity gradient. Test fractions were assayed for antiradical activities using electron spin resonance spectrometry, β-carotene-linoleate model and Folin-Ciocalteu assay; and antimicrobial activity against 2 Gram-negative bacteria, 4 Gram-positive bacteria and 2 fungal species using the disc diffusion assay. All fractions were also subjected to Fourier Transform Infrared (FTIR) analysis to identify types of functional groups present. It was found that the hydrophilic extracts (H2O fractions) possessed the most effective radical scavenging activity (p < 0.05) while the lipophilic extracts (PE fractions) the most active antimicrobial activity, especially against Gram-positive bacteria (p < 0.05). Total oxidation substrates content was found to be highest in the PE fractions of jellyfish bell and oral arms (p < 0.05). FTIR data showed that the H2O and MeOH fractions contains similar functional groups including -OH, -C=O, -N-H and -S=O groups, while the PE, DCM, and CHCl3 fractions, the -CH3, -COOH groups. This study showed that A. hardenbergi contains antioxidants and antimicrobials, thereby supporting the traditional claim of the jellyfish as an anti-aging and health-promoting functional food. Bioassay-guided fractionation approach serves as a critical milestone for the strategic screening, purification, and elucidation of therapeutically significant actives from jellyfish.

Bioequivalence Study of Toriem® Tablet to Motilium-M® Tablet (Domperidone Maleate 12.72 mg) Evaluated by Liquid Chromatography/Tandem Mass Spectrometry

  • Ryu, Ju-Hee;Choi, Sang-Jun;Lee, Myung-Jae;Lee, Jin-Sung;Kang, Jong-Min;Tak, Sung-Kwon;Seo, Ji-Hyung;Lee, Kyung-Tae
    • Journal of Pharmaceutical Investigation
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    • v.39 no.1
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    • pp.65-71
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    • 2009
  • The aim of the present study was to evaluate the bioequivalence of two domperidone maleate tablets, Motilium-$M^{(R)}$ Tablet (Janssen Korea Ltd., reference product) and $Toriem^{(R)}$ Tablet (Daewon Pharm. Co., Ltd., test product). Domperidone was extracted by liquid-liquid extraction using tert-butyl methyl ether and separated in less than 3 min on $C_{18}$ reverse-phase column using an isocratic elution. A tandem mass spectrometer, as detector, was used for quantitative analysis in positive mode by a multiple reaction monitoring mode to monitor the m/z $426.1{\rightarrow}119.1$ and the m/z $837.4{\rightarrow}158.2$ transitions for domperidone and the internal standard (roxithromycin), respectively. Calibration curves, from $0.05{\sim}50$ ng/mL of domperidone, showed correlation coefficients (r) higher than 0.9941. Intra day and inter day precision (C.V. %) for quality control were ranged from 10.04 to 16.09% and from 10.87 to 18.69%, respectively. The lower limit of quantification (LLOQ) of domperidone was 0.05 ng/mL. The method described is precise and sensitive and has been successfully applied to the study of bioequivalence of domperidone in 24 healthy Korean volunteers. Twenty-four healthy male Korean volunteers received a single dose of each medicine ($2{\times}12.72\;mg$ domperidone maleate) in a $2{\times}2$ crossover study. There was a one-week washout period between the doses. Plasma concentrations of domperidone were monitored for over a period of 24 hr after the administration. $AUC_{0-t}$ (the area under the plasma concentration-time curve) was calculated by the linear trapezoidal rule. $C_{max}$ (maximum plasma drug concentration) and $T_{max}$ (time to reach $C_{max}$) were compiled from the plasma concentration-time data. The 90% confidence intervals for the log transformed data were within acceptable range of log 0.8 to log 1.25 (e.g., $log\;0.92{\sim}log\;1.05$ for $AUC_{0-t}$, $log\;0.81{\sim}log\;1.05$ for $C_{max}$). The major parameters, $AUC_{0-t}$ and $C_{max}$ met the criteria of KFDA for bioequivalence indicating that $Toriem^{(R)}$ tablet is bioequivalent to Motilium-$M^{(R)}$ tablet.

Development of Simultaneous Analysis for the Multi-residual Pesticides in the Ginseng Extract using Gas Chromatography (인삼농축액에서 GC를 이용한 잔류농약 동시다성분 분석법의 개발)

  • Shin Yeong-Min;Lee Seon-Hwa;Son Yeong-Uk;Jeong Ji-Yoon;Jeoung Seoung-Wook;Park Heung-Jai;Kim Sung-Hun;Won Young-Jun;Lee Chang-Hee;Kim Woo-Seong;Hong Moo-Ki;Chae Kab-Ryong
    • Journal of Environmental Science International
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    • v.15 no.1
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    • pp.85-94
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    • 2006
  • The simultaneous analysis of multi-residual pesticides was developed using a gas chromatography (GC) method. In this study, a simple and reliable methodology was improved to detect 154 kinds of pesticides in sinseng extract sample by using a liquid-liquid extraction procedure, open column chromagraphy and chromatographic analysis by CC electron capture detector (ECD) and GC nitrogen-phosphorus detector (NPD). The 154 kinds of pesticides were classified in 4 groups according to the chemical structure. The extraction of pesticides was experimented with $70\%$ acetone and dichloromethane/petroleum ether in order, and cleaned up via open column chromatography $(3\times30cm)$ packed with florisil $(30g,\;130^{\circ}C,\;12hrs)$. The final extract was concentrated in a rotator evaporator at $40^{\circ}C$ until dryness. Then the residue was redissolved to 2ml with acetone, and analyzed by GC-ECD and GC-NPD. The applied concentration of pesticides was over $1\~10{\mu}g/ml$. The recovery tests were ranged from $70.7\%$ to $115.2\%$ with standard deviations between 0.3 and $5.7\%$ of the standard spiked to the ginseng extract sample (Group $I\~IV$). The limit of detection (LOD) ranged from 0.001 to $0.099{\mu}g/ml$ (Group $I\~IV$). The 9 kinds of pesticides were not detected. The developed method was applied satisfactory to the determination of the 154 kinds of pesticides in the ginseng extract with good reproducibility and accuracy.

Atomospheric Concentration and Mutagenicity of Nitroarenes of Suspended Particulates in Seoul (대기부유분진중 nitroarenes 오염도와 그 돌연변이원성에 관한 조사연구 - 서울시 일부지역을 중심으로 -)

  • Jo, Seong-Joon;Choi, Yong-Wook;Lim, Young-Wook;Shin, Dong-Chun;Chung, Yong
    • Environmental Analysis Health and Toxicology
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    • v.5 no.3_4
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    • pp.19-28
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    • 1990
  • Nitroarenes are ubiquitous environmental pollutants displaying potent mutagenicity in bacteria and carcinogenicity in mammal. In this study, the concentration of nitroarenes in coarse and fine particles and mutagenicity of POC$\_$N/ fraction was investigated in suspended particulates at the Shinchon and Bulkwang area of Seoul. The suspended particulates were collected bimonthly by a high volume cascade impactor air sampler from July 1987 to May 1988. Extractable organic matter was obtained by ultrasonic extraction on diethly ether/cyclohexane (8/2, v/v). Neutral fraction was obtained by liquid-liquid extraction. Polar neutral organic compounds (POC$\_$N/) was fractionated by thin-layer chromatography. Finally, the concentrations of nitroarenes in POC$\_$N/ fraction were measured and determined by capillary gas chromatography. Direct and indirect mutagenicity of POC$\_$N/ fraction were measured using Salmonella typhimurium TA 98. The result were as follows: 1) Major nitroarenes at the Shinchon area was 1-nitropyrene and at the Bulkwang area it was 2,7-dinitro-9-fluorenone during the year. 2) Average concentration of total nitroarenes measured was 67.26 ng/m$^3$in fine particles which was 1,3 folds higher that in coarse particle (52.30 ng/m$^3$). 3) Annual pattern of nitroarenes concentrations revealed that concentration during heating season (Feb., Jan., Mar.) was 2.2 folds higher than that in non heating season (May, Jul., Sep.). Concentration of each season has 157.68 ng/m$^3$and 80.39 ng/m$^3$. 4) The mutagenic activity of POC$\_$N/ fraction from fine particles was higher compared to that of coarse particles and was increased when metabolically activated, with 59 mixture. Mutagenicities, Metabolically activated, were significantly different between Shinchon and Bulkwang area, 322.8 rev/250 $\mu\textrm{g}$/plate and 286.8 rev/250 $\mu\textrm{g}$/plate, respectively. 5) Annual pattern of mutagenicity of POC$\_$N/ fraction revealed that mutagenicity during the heating season was 1.7 folds higher at Shinchon area and 1.2 folds higher at Bulkwang than during the non heating season. The variable contents and levels of nitroarenes in suspended particulates may affect human health significantly. Further studies such as risk assessment should be conducted on the basis of these kind of studies.

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Antioxidative Effects of Soybean Extracts by using Various Solvents (다양한 용매를 이용한 대두 추출물의 항산화효과)

  • Kim, Jee-Young;Maeng, Young-Sun;Lee, Ki-Young
    • Korean Journal of Food Science and Technology
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    • v.27 no.5
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    • pp.635-639
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    • 1995
  • The effective extraction of antioxidative substances from soybean was investigated by using various solvents, such as water, ethanol, methanol, acetone, chloroform, benzene, ethyl acetate, ether, dichloromethane, and hexane. Extraction was performed by cold method at $30^{\circ}C$ and by reflux method at $85^{\circ}C$. The antioxidative effect of the extracts was determined by peroxide value during the oxidation of soybean oil containing the extracts at $105^{\circ}C$ for 10 hours, and also by TBARS(thiobarbituric acid reactive substances) formed during the peroxidation of egg lecithin liposomes. The antioxidant activity of the extracts from raw soybean was higher than that from defatted soybean. The antioxidant activity of the extracts by reflux method was higher than that by cold method. The methanol extract from defatted and roasted soybean(DRS) showed the highest antioxidative effect against oxidation of soybean oil, while the water extract from DRS in egg lecithin liposomes. In the peroxidation of egg lecithin liposomes, the antioxidative effect of polar solvents extracts were higher than those by nonpolar solvents extracts.

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Rapid Gas Chromatographic Screening of Alcoholic Beverages for Volatile and Nonvolatile Organic Acids (기체크로마토그래피법에 의한 알코올 음료내 휘발성 및 비휘발성 유기산의 신속한 스크리닝)

  • Kim, Jung-Han;Kim, Kyoung-Rae;Chai, Jeong-Young;Park, Hyung-Kook;Choi, Kyoung-Sook
    • Korean Journal of Food Science and Technology
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    • v.26 no.2
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    • pp.162-166
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    • 1994
  • A rapid gas chromatographic (GC) profiling method for the simultaneous analysis of volatile and nonvolatile organic acids was applied to alcoholic beverages (white wine, red wine, brandy, and beer). It involves the solid-phase extraction of organic acids using Chromosorb P as the sorbent and diethyl ether as the eluent with subsequent triethylamine treatment. The resulting triethylammonium salts of acids were directly converted to volatile tert.-butyldimethylsilyl derivatives, which were analyzed by dual-capillary column GC and GC-mass spectrometry. From the alcoholic beverages studied, more than 29 organic acids were detected. When the simplified retention infer (RI) spectra of organic acids, and the direct comparisor method between alcoholic beverages and a test sample were attempted to identify a test sample, it was quickly recognized to be a red wine with the 998 ppt match quality value.

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Determination of the volatile flavor components of orange and grapefruit by simultaneous distillation-extraction (연속수증기증류추출법에 의한 오렌지와 자몽의 휘발성 유기화합물 확인)

  • Hong, Young Shin;Kim, Kyong Su
    • Food Science and Preservation
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    • v.23 no.1
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    • pp.63-73
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    • 2016
  • The volatile flavor components of the fruit pulp and peel of orange (Citrus sinensis) and grapefruit (Citrus paradisi) were extracted by simultaneous distillation-extraction (SDE) using a solvent mixture of n-pentane and diethyl ether (1:1, v/v) and analyzed by gas chromatography-mass spectrometry (GC-MS). The total volatile flavor contents in the pulp and peel of orange were 120.55 and 4,510.81 mg/kg, respectively, while those in the pulp and peel of grapefruit were 195.60 and 4,223.68 mg/kg, respectively. The monoterpene limonene was identified as the major voltile flavor compound in both orange and grapefruit, exhibiting contents of 65.32 and 3,008.10 mg/kg in the pulp and peel of orange, respectively, and 105.00 and 1,870.24 mg/kg in the pulp and peel of grapefruit, respectively. Limonene, sabinene, ${\alpha}$-pinene, ${\beta}$-myrcene, linalool, (Z)-limonene oxide, and (E)-limonene oxide were the main volatile flavor components of both orange and grapefruit. The distinctive component of orange was valencene, while grapefruit contained (E)-caryophyllene and nootkatone. $\delta$-3-Carene, ${\alpha}$-terpinolene, borneol, citronellyl acetate, piperitone, and ${\beta}$-copaene were detected in orange but not in grapefruit. Conversely, grapefruit contained ${\beta}$-pinene, ${\alpha}$-terpinyl acetate, bicyclogermacrene, nootkatol, ${\beta}$-cubebene, and sesquisabinene, while orange did not. Phenylacetaldehyde, camphor, limona ketone and (Z)-caryophyllene were identified in the pulp of both fruits, while ${\alpha}$-thujene, citronellal, citronellol, ${\alpha}$-sinensal, ${\gamma}$-muurolene and germacrene D were detected in the peel of both fresh fruit samples.

Extraction and effect of whitening agents from chinese plants (중국산 천연물에서 미백성분의 추출 및 효과)

  • Jin, Yinzhe;Li, Guanghua;Ahn, So Young;Kim, Eun-Ki;Row, Kyung Ho
    • Analytical Science and Technology
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    • v.19 no.3
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    • pp.194-202
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    • 2006
  • In this work, extraction and purification of the possible whitening agents from the Chinese plants; Chrysanthemum morifolium Ramat (xizang cai ju hua), Rhodiola sachalinensis, and Terminalia chebula Retzius have been described. The chopped leaves of Chrysanthemum morifolium Ramat and Terminalia chebula Retzius were added to water and ethyl ether, respectively. Components were separated on a GS310 column ($21.5{\times}500mm$ i.d., $10-15{\mu}m$) and concentrated into four or three portions. The chopped leaves of Rhodiola salientness were added to methanol and separated and concentrated on a column ($C_{18}$ column, $3.9^{\circ}$�F8;300 mm i.d., $15{\mu}m$) into two parts. The whitening effects of extracts were examined by in-vitro melanin production assay, in melana and B16 cells at a concentration of $10{\mu}g/ml$. The ethyl acetate layer of Chrysanthemum morifolium Ramat showed 92% melanin inhibitory at $200{\mu}g/ml$, the extract of Rhodiola sachalinensis showed a whitening effect of about 60% melanin inhibitory, which was more efficient than the whitening effect of arbutin (45.6%). The methanol extract of Terminalia chebula Retzius inhibited melanin expression by 90% at $100{\mu}g/ml$; however, it was toxic to B16 melanoma cells.

Inhibitory Effect against Angiotensin Converting Enzyme and Antioxidant Activity of Panax ginseng C. A. Meyer Extracts (인삼 추출물의 Angiotensin Converting Enzyme 저해 효과와 항산화 활성)

  • Lee, Seung-Eun;Seong, Nak-Sul;Bang, Jin-Ki;Kang, Seung-Won;Lee, Sung-Woo;Chung, Tae-Yung
    • Korean Journal of Medicinal Crop Science
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    • v.11 no.3
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    • pp.236-245
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    • 2003
  • The study was performed for elucidating angiotensin converting enzyme (ACE) inhibitory activity and comparing antioxidative activity of Panax ginseng extracts prepared at different conditions. Total phenolic content, inhibitory activity on ACE and antioxidative effects were tested on 10 ethanolic extracts and correlation coefficient between total phenolic content and physiological activity was calculated. Yield and total phenolic content of 50% ethanolic extract prepared at $85^{\circ}C$ exhibited the highest value as 42.52% and 0.82%, respectively. Among the fractions obtained from 50% ethanolic extract prepared at room temperature, water fraction showed the highest value in yield as 72.08% and ethyl acetate fraction did in total phenolic content as 6.59%. In the test on ACE inhibitory activity, 50% ethanolic extract obtained at room temperature indicated the strongest effect of 93.8% which was higher than 85.2% of commercialized ACE inhibitor and solvent fractions showed potent inhibitory activity in order of hexane fraction, diethyl ether fraction, ethyl acetate fraction, butanol fraction and water fraction at concentration of $4000{\mu}g/ml$. 50% Ethanolic extract prepared at $85^{\circ}C$ had the most potent inhibition effect on human LDL oxidation as 78.2% at $200{\mu}g/ml$ and the other extracts also did above 60%. Diethyl ether fraction and ethyl acetate fraction showed strong inhibition activity $(34.38%{\sim}78.13%)$ on LDL oxidation at concentration of $10{\sim}200\;{\mu}g/ml$. From the statistical analysis via SAS program, correlation coefficient between total phenolic content and ACE inhibitory effect was 0.6353 at P<0.05. Conclusively, this report showed that the most efficient extraction condition for elevating inhibitory activity on ACE and LDL oxidation, phenolic content and yield from Panax ginseng was 50% ethanol extraction at room temperature or high temperature condition. And Panax ginseng would be used for preventing hypertension or atheroscrelosis for man via inhibitory action on ACE and LDL oxidation.

Determination of finasteride in human serum by LC-MS/MS (LC-MS/MS를 이용한 혈청 중 finasteride 분석)

  • Nam, Hye-Seon;Nam, Kyong-Hee;Jung, Su-Hee;Lee, Jang-Woo;Kang, Jin-Yeong;Hong, Soon-Keun;Kim, Tae-Sung;Kang, Tae-Seok;Yoon, Hae-Jung;Lee, Kwang-Ho;Rhee, Gyu-Seek
    • Analytical Science and Technology
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    • v.24 no.5
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    • pp.345-351
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    • 2011
  • A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed and validated for the determination of finasteride in human serum. Beclomethasone was used as internal standard (IS) and liquid-liquid extraction (LLE) using methyl tert-butyl ether (MTBE) was carried out to isolate analyte. The mass transitions monitored in multiple reaction monitoring (MRM) in positive ion mode were m/z 373.2${\rightarrow}$305.2 for finasteride and m/z 409.3${\rightarrow}$391.2 for IS. Retention times of finasteride and IS were 5.81 and 5.46 min, respectively. The limit of quantitation (LOQ) was 0.1 ng/mL and the calibration curve showed good linearity in the range of 0.1~20.0 ng/mL ($R^2$=0.9997). The intra-day assay precision and accuracy were in the range 6.3~10.6% and 97.3~103.6%, respectively, and the inter-day assay precision and accuracy were in the range 0.8~5.2% and 99.8~102.5%, respectively. The sample extract recovery of the method was 80~83%.