• Title/Summary/Keyword: ether extraction

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A Sensitive, Efficient, and Cost-Effective Method to Determine Rotigotine in Rat Plasma Using Liquid-Liquid Extraction (LLE) and LC-MRM

  • Kim, Ji Seong;Jang, Yong Jin;Kim, Jin Hee;Kim, Jin Hwan;Seo, Jae Hee;Park, Il-Ho;Kang, Myung Joo;Choi, Yong Seok
    • Mass Spectrometry Letters
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    • v.13 no.4
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    • pp.146-151
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    • 2022
  • Rotigotine (RTG) is a non-ergot dopamine agonist used to manage the early stage of Parkinson's disease (PD) as transdermal patch. However, the poor medication compliance of PD patients and skin issues related with repeated applications of RTG patches lead to the search for alternative formulations and it also requires appropriate analytical methods for their in vivo evaluation. Thus, here, a sensitive, efficient, and cost-effective method to determine RTG in rat plasma using liquid-liquid extraction (LLE) and multiple reaction monitoring was developed. The use of 20 µL of rat plasma for sample treatment, 8-OH-DPAT as the internal standard, and methyl tert-butyl ether as the LLE solvent in the present method gives it advantages over previous methods for the analysis of RTG in biological samples. The good analytical performance of the developed method was confirmed in specificity, linearity (the coefficient of determination ≥0.999 within 0.1-100 ng/mL), sensitivity (the lower limit of quantitation at 0.1 ng/mL), accuracy (81.00-115.05%), precision (≤10.75%), and recovery (81.00-104.48%) by following the FDA guidelines. Finally, the applicability test of the validated method to the in vivo evaluation of a RTG formulation showed that the present method is the only method which can be accurately applied to that longer than 24 hours, critical for the development of formulations with reduced dosing frequencies. Therefore, the present method could contribute to the development of new RTG formulations helpful to people suffering from PD.

The Solvent Extraction of Univalent Cation Picrates by New Podands (새로운 포단드에 의한 피크린산 일가 양이온 염의 용매추출)

  • Jung, Jong Hwa;Cho, Sung Bae;Kim, Jineun;Kim, Jae Sang;Lee, Shim Sung
    • Analytical Science and Technology
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    • v.6 no.1
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    • pp.29-37
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    • 1993
  • Some new podands containing phenyl(B), benzyl(Bz), pyridine(Py), quinoline(Q) and naphthalene(Np) as end-groups, and oxygen(O) and sulfur(S) in ether chains as donor atoms have been synthesized. The univalent cation binding characteristics of these podands have been studied by NMR titration and solvent extraction. By NMR titration we have found that the most of podands form 1:1 complexes with $Ag^+$ ion. Especially, the substituted sulfur atoms in ether chains show the effects to enhance the stabilities. We also carried out the extractions of univalent cation picrates including alkaline metal, $Ag^+$, $Tl^+$ and $NH_4{^-}$ ions from aqueous to chloroform layer by using these podands. We found that the extractabilities of $Ag^+$ ion with the quinoline-containing podands such as, $Q_2O_4$, $Q_2O_5$ and $BQO_5$ were 86.8, 86.6 and 48.0% respectively, but the naphthalene-containing podands such as, $Np_2O_4$ and $Np_2O_5$ extracted quite small amount. Otherwise, in cases of $Bz_2O_3S_2$(89.4%), $B_2O_2S_2$(96.8%), $B_2O_3S_2$(58.9%), $Py_2O_2S_2$(58.8%), $Py_2O_3S_2$(42.1%), and $B_2O_4S$(15.0%), interestingly, $Bz_2O_3S_2$ which have sulfur atoms and benzyl groups showed the highest extraction selectivity for $Ag^+$ ion. This result seems due to not only the strong interaction of $Ag^+$ ion with sulfur donors according to the HSAB theory, but also the effective ${\pi}-{\pi}$ stacking interaction between two aromatic end-groups which is enhanced by the flexible methylene spacing group in benzyl groups instead of phenyl groups. The extraction coefficients gave the similar tendency as the extractabilities and the stabilities. From these results, it could be concluded that the predominant factor affected to extraction coefficients is the stabilities, which are strongly influenced by the structures of podands.

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New Methods for Isolation of Sesquiterpene from Panax ginseng (인삼 Sesquiterpene의 새로운 분리방법)

  • 위재준;신지영
    • Journal of Ginseng Research
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    • v.21 no.3
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    • pp.214-218
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    • 1997
  • New simple methods for the Isolation of sesquiterpenes from Panax ginseng were developed. First, volatile compounds were isolated by simultaneous distillation and extraction (SDE) with 30% methanol and $\alpha$-hexane instead of water and ethyl ether/pentane (1:1). Secondly, head space volatiles in U-shaped tube at 7$0^{\circ}C$ were passed through C18 Sep-Pak by nitrogen gas streaming and the adsorbed volatiles were fluted by $\alpha$-hexane. TLC analysis showed that the volatile concentrates consisted mainly of terpenes when colored by vanillin-sulfuric and. GC/MS data revealed that approximately 30 sesquiterpenes of molecular weight 204 occupied 81.1% or more of the volatile concentrates isolated by those two newly developed methods. Among these, alloaromadendrene, germacrene B, isocaryophyllene, $\alpha$-neoclovene, ${\gamma}$-muurolene, $\beta$-panaslnsene, and $\alpha$-humulene were identified as being major sesqulterpenes by authentic samples or literatme search Key words : Panax ginseng, volatile compound, sesquiterpene, isolation, new method, GC/MS.

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Antioxidative Activity of Various Solvent Extracts of Quercisemen to Linoleic Acid (상수리(상실(橡實))의 각종 용매 추출물이 linoleic acid의 항산화력에 미치는 영향)

  • Sin, Du-Ho;Jo, Jeong-Sun
    • Journal of the Korean Applied Science and Technology
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    • v.8 no.1
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    • pp.79-83
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    • 1991
  • The extracts of Quercisemen(Quereus acutissima Carruthers seed) powder was obtained by the extraction with distilled water, water : acetonet(1:1, v/v), ethanol and ethyl ether, respectively. As a result this experiment, the antioxidative activity of each solvent extracts on linoleic acid were examined as follows: 1. Each fraction extracted by the acetone : water(1:1, v/v), water and ethanol respectively showed high antioxidative activity. 2. A fraction of the tannin extracted from the solvent, acetone, water(1:1, v/v) showed even more antioxidative activity than that of the ${\alpha}$-tocopherol or BHT. 3. Acceleration of peroxide reaction by $Fe^{++}$ and $Cu^{++}$ on the linoleic acid was strongly inhibited by adding the tannin, 4. Organic acid, such as malic acid, citiric acid and tartaric acid with the tannin were showed the synergistic effect fo the antioxidation reaction.

Separation and Purification of Cholesterol from By-product of Low Cholesterol Egg Yolk (저콜레스테롤 난황 제조시 생성되는 부산물로부터 콜레스테롤의 분리 정제)

  • 유익종;조혜연;박우문;전기홍;최성유
    • Food Science of Animal Resources
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    • v.20 no.1
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    • pp.36-43
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    • 2000
  • $\beta$-cyclodextrin adsorption and saponification methods were applied to isolate and purify cholesterol from the by-product of the low-cholesterol egg yolk product. They by-product was prepared from processing low-cholesterol egg yolk followed by extracting with chloroform to remove $\beta$-cyclodextrin and concentrated to 3,069 mg% cholesterol. When $\beta$-cyclodextrin method between two purification methods was applied, 50% ethanol as a solvent showed higher cholesterol concentration of 5.82% rather than the other solvents. Repeated purification of 3 times could not improve the cholesterol concentration significantly(p<0.05). In case of purification using saponification method, hexane as a solvent for extraction of unsaponificated materials was more efficient to increase cholesterol concentration than chloroform and ether. 60 times(v/w) saponification solution (95% ethanol:33% KOH = 94:6) of sample weight was most effective to increase the cholesterol concentration of 35.7%. Repeated purification process by saponification method could increase cholesterol concentration to 95.7% by 4 times repetition.

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The Study on the Composition in Pharmacopunctures of Eight Principles by Gas Chromatography/Mass Spectrometry (Gas Chromatography/Mass Spectrometry를 이용한 팔강약침액 성분에 대한 연구)

  • Kim, Hyub;Ahn, Byung-Soo
    • Journal of Pharmacopuncture
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    • v.11 no.3
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    • pp.79-91
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    • 2008
  • Objective: The purpose of this study was to investigate the composition for pharmacopunctures of eight principles hydrodistillation layer. Methods: The study was determined the hydrodistillation layer for pharmacopunctures of eight principles by hydrodistillation method. The effective components in hydrodistillation layer for pharmacopunctures of eight principles were extracted with ethyl ether or dichloromethane, and then analyzed by Gas Chromatography/Mass Spectrometry(GC/MS). Results: 1. Analyzed pharmacopunctures of eight principles by GC/MS, a lot of differences according to extraction solvent by each pharmacopunctures of eight principles and specific peak patterns were seen. 2. The main compound in pharmacopunctures of eight principles was a kind of hexaoxacyclohydrocarbon that has long hydrocarbon chain.

Studies on Constituents of Higher Fungi of Korea(XL) - A Sterol of Phallus impudicus - (한국산(韓國産) 고등(高等) 균류(菌類)의 성분(成分) 연구(硏究)(제40보)(第40報) - 말뚝버섯의 스테롤 성분(成分) -)

  • Choi, Eung-Chil;Chung, Kyeong-Soo;Kim, Jong-Chan;Kim, Byong-kak
    • The Korean Journal of Mycology
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    • v.11 no.2
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    • pp.97-98
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    • 1983
  • The carpophores of Phallus impudicus collected at Gal-mae-ri in Gyeong-gi Province were subjected to chemical analysis for sterol constituents. The dried carpophores were homogenized and extracted with chloroform-methanol(2 : 1). After saponification of the dried extract, unsaponified components were obtained by ether extraction of the reaction mixture. A sterol fraction was separated by preparative TLC and from this fraction, ergosterol was identified by gas­chromatographic analysis with authentic sterols.

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Drying Characteristics of Garlic (마늘의 건조특성에 관한 연구)

  • 이정호;고학균
    • Journal of Biosystems Engineering
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    • v.21 no.1
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    • pp.72-83
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    • 1996
  • This study was performed to find out drying characteristics and develop drying model for the design of an efficient dryer or drying system of garlic. The basic model which describes drying phenomenon of garlic was first established. A series of drying test were conducted with two varieties of garlic(Uiseong, Namdo) at 9-different drying conditions (drying temperatures ; $40^{\circ}C$, $50^{\circ}C$, $60^{\circ}C$, relative humidities ; 20%, 35%, 50%) and statistical analysis was made to fit the data with exponential equation, approximated diffusion equation, page equation, thompson equation and wang equation, respectively. In this test, the effects of drying air temperature and relative humidity on the drying rate were undertaken. Finally, new drying model based on these experimental results was developed to describe the drying characteristics of garlic. Also, the volatile components of garlic extracts were investigated. For experiment both Uisoeng and Namdo garlic were dried by heated-air-drying, followed by ether extraction. The extracts were analysed by Gas chromatography/Mass spectrometer.

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Effect of Butanol Extracts from Prunus mume on the Growth of Salmonella typhimurium (오매의 Butanol추출물이 Salmonella typhimurium의 생육에 미치는 영향)

  • 서명희;배지현
    • Journal of Nutrition and Health
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    • v.35 no.9
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    • pp.926-931
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    • 2002
  • The antimicrobial properties of extracts of Prunus mume were tested on Salmonella paratyphimurium and S. typhimurium. First, the Prumus mume was extracted with methanol at several temperatures, and then fractionation of the methanol extracts from Prunus mume was carried out by using petroleum ether, chloroform, ethyl acetate or butanol. Secondly, absorption column chromatoraphy (using a Diaion HP 20) was conducted to eliminate some water soluble materials that might inhibit the antimicrobial activity of some extracts. The antimicrobial activitry of each of the Prunus mume extracts was determined using a paper disc method against several food-borne pathogens, The growth inhibition curve was determine using butanol extracts of Prunus mume against Salmonella typhimurium. The extraction temperature did not have any significant effect on the yield of the extract or on the level of antimicrobial activity. The butanol extract of Prunus mume showed strong antimicrobial activity against Salmonella paratyphimurium and S. typhimurium; a 1,000 ppm of butanol extract of Prunus mume retared the growth of S. typhimurium up to 36 hours. (Korean J Nutrition 35(9) : 926~931, 2002)

Analysis of 4-Nitrotoluene in Water by Gas Chromatography/Mass Spectrometry (기체크로마토그래피/질량분석기에 의한 수질시료 중 4-니트로톨루엔의 분석법 연구)

  • 이희경;권오승;류재천
    • Environmental Analysis Health and Toxicology
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    • v.15 no.1_2
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    • pp.45-51
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    • 2000
  • Analytical method of 4-nitrotoluene (4-NT) in water was developed by 9as chromatography/mass selective detector/selected ion monitoring (GC/MSD/SIM). 4-NT was extracted with diethyl ether. Organic layer was washed with 5 % sodium chloride solution. The influence of solvent and evaporation condition on extraction of 4-NT were examined. The retention time of 4-NT peak was 7.72 min. Coefficient of variation (CV) of 4-NT (ng) within day and day-to-day was ranged from 7.0 to 14.6% and from 7.7 to 20.8%, respectively. Recovery of 4-NT was ranged from 84 to 109%, and detection limit of 4-H was lese than 1 ng/㎖.

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