• Title/Summary/Keyword: ether extraction

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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%.

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

  • Nam, Hye-Seon;Nam, Kyong-Hee;Jung, Su-Hee;Lee, Jang-Woo;Kang, Jin-Yeong;Hong, Soon-Keun;Kim, Tae-Sung;Jung, Ki-Kyung;Kang, Tae-Seok;Yoon, Hae-Jung;Lee, Kwang-Ho;Rhee, Gyu-Seek
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.76-82
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    • 2012
  • The determination and confirmation of dutasteride in human serum was performed by a liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS). Beclomethasone as an internal standard (I.S.) was added to the serum and the mixed sample was pretreated by liquid-liquid extraction (LLE) with methyl tert-butyl ether (MTBE). The mass transitions of dutasteride and I.S. monitored in multiple reaction monitoring (MRM) were m/z 529.6${\rightarrow}$461.5 and m/z 409.3${\rightarrow}$391.2, respectively, and the retention times were 6.45 and 5.46 min, respectively. The calibration curve was linear in the concentration range of 0.5~30.0 ng/mL ($R^2$= 0.9999) and the limit of quantitation (LOQ) was found to be 0.5 ng/mL. The recovery of dutasteride was shown to be 66~72%. The intra-day assay precision and accuracy were in the range 3.5~5.5% and 85.7~89.9%, respectively, and the interday assay precision and accuracy were in the range 4.2~5.8% and 90.8~95.8%, respectively.

Development of a Simultaneous Analysis Method for DDT (DDD & DDE) in Ginseng (인삼 중 DDT(DDD 및 DDE) 분석법의 개발)

  • Kim, Sung-Dan;Cho, Tae-Hee;Han, Eun-Jung;Park, Seoung-Gyu;Han, Chang-Ho;Jo, Han-Bin;Choi, Byung-Hyun
    • Korean Journal of Food Science and Technology
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    • v.40 no.2
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    • pp.123-128
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    • 2008
  • The MRLs (maximum residue limits) of DDT (DDD and DDE) in fresh ginseng, dried ginseng, and steamed red ginseng are set as low as 0.01 mg/kg, 0.05 mg/kg, and 0.05 mg/kg, respectively. Therefore, this study was undertaken to develop a simple and highly sensitive analysis method, as well as to reduce interfering ginseng matrix peaks, for the determination of DDT isomers (o,p'-DDE, p,p'-DDE, o,p'-DDD, p,p'-DDD, o,p'-DDT, and p,p'-DDT) in fresh ginseng, dried ginseng, and steamed red ginseng at the 0.01 mg/kg level. The method used acetonitrile extraction according to simultaneous analysis, followed by normal-phase Florisil solid-phase extraction column clean-up. The purification method entailed the following steps: (1) dissolve the concentrated sample extract in 7 mL hexane; (2) add 3 mL of $H_2SO_4$; (3) vigorously shake on avortex mixer; (4) cetrifuge at 2000 rpm for 5 min; (5) transfer 3.5 mL of the supernatant to the Florisil-SPE (500 mg/6 mL);and (6) elute the SPE column with 1.5 mL of hexane and 10 mL of ether/hexane (6:94). The determination of DDT isomers was carried out by a gas chromatography-electron capture detector (GC-${\mu}$ECD). The hexane and ether/hexane (6:94) eluate significantly removed chromatographic interferences, and the addition of 30% $H_2SO_4$ to the acetonitrile extract effectively reduced many interfering ginseng matrix peaks, to allow for the determination of the DDT isomers at the 0.01 mg/kg level. The recoveries of the 6 fortified (most at 0.01 mg/kg) DDT isomers from fresh ginseng, dried ginseng, and steamed red ginseng ranged from 87.9 to 99.6%. The MDLs (method detection limits) ranged from 0.003 to 0.009 mg/kg. Finally, the application of this method for the determination of DDT isomers is sensitive, rapid, simple, and inexpensive.

Effects of the Substances Extracted from Dried Mushroom(Lentinus edodes) by Several Organic Solvents on the Stability of Fat (건조(乾燥)표고버섯의 각종(各種) 용매추출물(溶媒抽出物)의 항산화작용(抗酸化作用)의 효과(效果))

  • Ma, Sang-Jo
    • Korean Journal of Food Science and Technology
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    • v.15 no.2
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    • pp.150-154
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    • 1983
  • Mushroom, Lentinus edodes which had been dried at $50^{\circ}C$ for 20 hours were extracted with small amount of ethanol, methanol, chloroform and petroleum ether, respectively. The extracts were then dissolved in edible soybean oil, and the resulting substrates and a portion of the soybean oil (control) were placed in an incubator $(37.0{\pm}1.0^{\circ}C)$ for eight weeks. Peroxide values and TBA values of control and the substrates were determined regularly during the storage period. The results of the present study were as follows: 1. The moisture contents of the mushroom which was 84.88% on wet basis at the time of harvest were reduced to 15.12% after drying. 2. Extracts obtained from alcohols were effective in retarding the POV development. 3. There was not much difference among the TBA values after 14 days, but significant difference of the TBA values in control and the substrates extracts were observed in longer storage period TBA values of substrate containing ethanol and methanol in the later stage period were smaller than that of the substrates containing petroleum ether and chloroform. 4. In view of the POV and TBA value development, ethanol and methanol were more effective solvents for the extraction of antioxidant compounds in the dried mushroom than chloroform and petroleum ether.

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Analysis of volatile compounds and metals in essential oil and solvent extracts of Amomi Fructus (사인으로부터 추출한 정유와 용매 추출물의 휘발성 물질 및 금속성분 분석)

  • Lee, Sam-Keun;Eum, Chul Hun;Son, Chang-Gue
    • Analytical Science and Technology
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    • v.28 no.6
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    • pp.436-445
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    • 2015
  • Amomi Fructus with anti-oxidative activity was chosen and essential oil was obtained by SDE (simultaneous distillation extraction), and 39 constituents were determined by GC-MS (gas chromatography-mass spectrometry). Major components were camphor, borneol acetate, borneol, D-limonene and camphene. Three solvent extracts such as hexanes, diethyl ether and methylene chloride from Amomi Fructus were obtained. These were analyzed by GC-MS and 4 more constituents were identified in addition to 39 components discovered in essential oil. Five major components such as camphor, borneol acetate, borneol, D-limonene and camphene were also detected, however the relative peak percents of those components were different from those of constituents in essential oil. To estimate the kind and the amount of materials evaporated at certain temperature and conditions from essential oil and solvent extracts, dynamic headspace apparatus was used and materials evaporated and trapped at certain conditions were analyzed by GC-MS. Recovery yield of SDE method from Amomi Fructus was measured by using camphor and standard calibration solution of camphor methanol solution and, the yield was 82.0%. Content of Hg was measured by mercury analyzer and contents of Cd, Pb, Cr, Mn, Co, Ni, Cu and Zn in Amomi Fructus, essential oils and solvent extracts were determined by ICP-MS (Inductively coupled plasma-mass spectrometer). Pb, Cd and Hg were measured in the concentration of 0.72 mg/kg, <0.10 mg/kg and 0.0023 mg/kg, respectively and these were below permission level of purity test. Contents of Mn, Cu and Zn in Amomi Fructus were 213 mg/kg, 8.29 mg/kg and 31.0 mg/kg, respectively and which were relatively higher than other metals such as Cr, Co and Ni. Metals such as Mn (0.65 ~ 9.08 mg/kg), Cu (1.16 ~ 4.40 mg/kg) and Zn (1.10 ~ 3.80 mg/kg) in essential oil and solvent extracts were detected. At this point it is not clear that the metals were cross-contaminated in the course of treating Amomi Fructus or metals were contained in Amomi Fructus. The influence evaluation toward biological model study of these metals in essential oil and solvent extracts will be needed.

Method Development for the Profiling Analysis of Endogenous Metabolites by Accurate-Mass Quadrupole Time-of-Flight(Q-TOF) LC/MS (LC/TOFMS를 이용한 생체시료의 내인성 대사체 분석법 개발)

  • Lee, In-Sun;Kim, Jin-Ho;Cho, Soo-Yeul;Shim, Sun-Bo;Park, Hye-Jin;Lee, Jin-Hee;Lee, Ji-Hyun;Hwang, In-Sun;Kim, Sung-Il;Lee, Jung-Hee;Cho, Su-Yeon;Choi, Don-Woong;Cho, Yang-Ha
    • Journal of Food Hygiene and Safety
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    • v.25 no.4
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    • pp.388-394
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    • 2010
  • Metabolomics aims at the comprehensive, qualitative and quantitative analysis of wide arrays of endogenous metabolites in biological samples. It has shown particular promise in the area of toxicology and drug development, functional genomics, system biology and clinical diagnosis. In this study, analytical technique of MS instrument with high resolution mass measurement, such as time-of-flight (TOF) was validated for the purpose of investigation of amino acids, sugars and fatty acids. Rat urine and serum samples were extracted by selected each solvent (50% acetonitrile, 100% acetonitrile, acetone, methanol, water, ether) extraction method. We determined the optimized liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) system and selected appropriated columns, mobile phases, fragment energy and collision energy, which could search 17 metabolites. The spectral data collected from LC/TOFMS were tested by ANOVA. Obtained with the use of LC/TOFMS technique, our results indicated that (1) MS and MS/MS parameters were optimized and most abundant product ion of each metabolite were selected to be monitorized; (2) with design of experiment analysis, methanol yielded the optimal extraction efficiency. Therefore, the results of this study are expected to be useful in the endogenous metabolite fields according to validated SOP for endogenous amino acids, sugars and fatty acids.

Effect of antioxidation and antibacterial activity on crude extract and Characterization of American Cockroaches (Periplaneta americana L.) in Korea (국내 서식 미국바퀴(Periplaneta americana L.)의 특성 및 추출물의 항산화·항균 효과)

  • Kim, Jung-Eun;Kim, Seon-Gon;Kang, Sung-Ju;Kim, Chun-Sung;Choi, Yong-Soo
    • Journal of Sericultural and Entomological Science
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    • v.53 no.2
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    • pp.135-142
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    • 2015
  • The American cockroaches, Periplaneta americana L. was the most important worldwide pest species. It has been an public health problems. We were determinated life cycle and extraction of crude extracts by chemical reagents from cockraches (P. americana L.). The extracted crude solution has been antibacterial activity to gram negative bacteria (Pseudomonas aeruginosa, $6.44{\pm}1.03mm$), gram positive bacteria (Bacillus subtilis, $1.88{\pm}0.40mm$), and fungus (Candida albicans, $5.61{\pm}0.57mm$) using radial diffusion assay. We were analysed of up-regulation of Glutathione-S-transferases (GSTs) stimulation, indicating that antioxidantial protein from various classes are simultaneously expressed in a single insect upon infection or injury. The gene from Periplaneta americana L. were cloned, analysed sequence, and measured protein expression by Real Time PCR (Polymerase Chain Reaction).

Distribution of Cadmium in a Strain of Staphylococcus aureus Resistant Against the Metal (카드뮴내성(耐性) Staphylococcus aureus내(內) 카드뮴분포(分布))

  • Hyun, Eun-Min;Park, Chan-Seung;Choi, Kyoung-Ho
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.10 no.1
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    • pp.103-106
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    • 1981
  • A strain of Staphylococcus aureus resistant against cadmium was cultivated by using a liquid medium containing 10ppm cadmium ion, and then, it was fractionated into several fractions as described in the previous paper. Content of the metal in each fraction was determined through an atomic absorption spectrometery. The results are as follows; (1) A $690.9{\mu}g$ cadmium was contained in one gram dry cell. (2) A 39.9% of total cadmium was easily extracted by TCA, however a 52.2% was unextractable even by series of extraction with TCA, ethanol-ehter, perchloric acid and ammonium water. (3) Among the fractions prepared along the cellular structure, plasma membrane fraction showed a highest content of the metal by containing a 59.1%. (4) The fraction of cytoplasm and cell wall contained a 26.8 and 14.1%, respectively. (5) More than 90% of the metal contained in the cell wall was detected from the fraction of lipopolysaccharide. It is considered from these results tht at least a 70% of the cadmium up taken by the resistant cell associates with membranous structure in the cell surface.

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Relationship between Weather Factors and Chemical Components of Flue-cured Tobacco (기상요인과 황색종 잎담배의 화학성분과의 관계)

  • Kim Sang-Beom;Cho Soo-Heon;Chung Youl-Young;Jeong Kee-Taeg
    • Journal of the Korean Society of Tobacco Science
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    • v.26 no.2 s.52
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    • pp.93-101
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    • 2004
  • This study was conducted to investigate the relationship between weather factors during the growing season and chemical components of flue-cured tobacco. Chemical components used in this study was from 'Farm Leaf Tobacco Test' conducted at KT&G Central Research Institute from 1986 through 2003. Data of weather factors during growing season(April to July) were collected in 10 districts measured at Korea Meteorological Adminstration(KMA). Nicotine and total sugar contents, and total sugar to nicotine(TS/Nic.) ratio were increased, whereas total nitrogen to nicotine(TN/Nic.) ratio and chloride content were decreased from 1986 through 2003. Year to year variation of rainfall was the largest, followed by that of sunshine hour. Month to month variation of rainfall also was the largest, followed by that of mean daily air temperature(MDAT). Rainfall was correlated positively with relative humidity(RH), but negatively with sunshine hour. Nicotine content was correlated positively with MDAT(in July, June$\~$July, May$\~$July and average), but negatively with rainfall(in May$\~$July) and with RH(in June, July, May $\~$June, June $\~$July, April$\~$June, May $\~$July and average). Total sugar content was correlated positively with MDAT(in May), but negatively with sunshine hour(average) and RH(in June, July, June$\~$July, April$\~$June, May$\~$July and average). The positive correlation was found between total nitrogen content and sunshine hour(in April, May, April$\~$May, May$\~$July, April$\~$June and average). The negative correlation was found between TS/Nic. ratio and sunshine hour(in May$\~$July and average). TN/Nic. ratio was correlated positively with sunshine hour(in May and April$\~$May) and with RH(in July and June$\~$July), but negatively with MDAT(in July, June$\~$July, May$\~$July and average). Ether extraction content was correlated positively with MDAT(in July, June$\~$July, May$\~$July and average) and with sunshine hour(in July and June$\~$July), but negatively with rainfall(in April, July, May­July and average). Chloride content was correlated positively with sunshine hour(in April, July, April$\~$May, June$\~$July, April$\~$June, May$\~$July and average), but negatively with rainfall(in April, April$\~$June and average).