• Title/Summary/Keyword: Various solvent extraction

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GC/MS Analysis of Ethylene Glycol in the Contaminated Lubricant Oil Through Solvent Extraction Followed by Derivatization using Bistrimethylsilyltrifluoroacetamide (BSTFA) (엔진윤활유 중 Ethylene Glycol의 용제추출후 bistrimethylsilyltrifluoroacetamide(BSTFA)를 이용한 GC/MS 분석에 관한 연구)

  • Lee, Joon-Bae;Kwon, O-Seong;You, Jae-Hoon;Shon, Shungkun;Sung, Tae-Myung;Paeng, Ki-Jung
    • Tribology and Lubricants
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    • v.28 no.6
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    • pp.315-320
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    • 2012
  • For proper functioning, general machines usually need lubricant oil as a cooling, cleaning, and sealing agent at points of mechanical contact. The quality of lubricant oil can deteriorate during operation owing to various causes such as high temperature, combustion products and extraneous impurities. In this study, a heavy load stopped during operation, and the oil was analyzed to check whether any impurities were added. Extraction using acetonitrile followed by reaction with BSTFA(bistrimethylsilyl trifluoroacetamide) showed that, trimethylsilylated ethylene glycol was present in the lubricant oil. To quantify the ethylene glycol in the oil, deuterium-substituted ethylene glycol, which acted as an internal standard, was added to the sample and then extracted with the solvent. Next, the extract was reacted with the derivatizing agent(BSTFA) and then analyzed with GC/MS. The detection limit of this method was found to be $0.5{\mu}g/g$ and the recovery of oil containing $20,000{\mu}g/g$ of ethylene glycol was measured to be 94.8%. A damaged O-ring and eroded cylinder liner were found during the overhaul, which implied the leakage of coolant containing ethylene glycol into the lubricating system. The erosion of the cylinder liner was assumed to be due to cavitation of the coolant in the cooling system.

Identification of the Antibiotic-Producing Chstridium sp. KH-431 and Purification of the Antibiotics (항생물질을 생산하는 Clostridium sp. KH-431의 동정 및 항생물질의 정제)

  • 홍수형;김미정;박용복;이재근;하지홍
    • Microbiology and Biotechnology Letters
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    • v.21 no.1
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    • pp.41-46
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    • 1993
  • A strain showing antibiotic activities against various bacteria and fungi was selected from approximately 2,000 microorganisms obtained from soil samples. This strain, designated as KH-431, was identified as a Clostridium sp. by its morphological, physiological and biochemical characteristics. The highest production of the antibiotics was achieved in a fermentation medium containing sorbitol, yeast extract, d-biotin and $CaCl_2$ The antibiotics were isolated from the culture broth by solvent extraction using ethyl acetate, silica gel column chromatography and recrystallization. Two kinds of antibiotics, KG-431A and KG-431B were obtained after the purification procedure, and only KG-431B was successful to recrystallize.

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Fates of water and salts in non-aqueous solvents for directional solvent extraction desalination: Effects of chemical structures of the solvents

  • Choi, Ohkyung;Kim, Minsup;Cho, Art E.;Choi, Young Chul;Kim, Gyu Dong;Kim, Dooil;Lee, Jae Woo
    • Membrane and Water Treatment
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    • v.10 no.3
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    • pp.207-212
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    • 2019
  • Non-aqueous solvents (NASs) are generally known to be barely miscible, and reactive with polar compounds, such as water. However, water can interact with some NASs, which can be used as a new means for water recovery from saline water. This study explored the fate of water and salt in NAS, when saline water is mixed with NAS. Three amine solvents were selected as NAS. They had the same molecular formula, but were differentiated by their molecular structures, as follows: 1) NAS 'A' having the hydrophilic group ($NH_2$) at the end of the straight carbon chain, 2) NAS 'B' with symmetrical structure and having the hydrophilic group (NH) at the middle of the straight carbon chain, 3) NAS 'C' having the hydrophilic group ($NH_2$) at the end of the straight carbon chain but possessing a hydrophobic ethyl branch in the middle of the structure. In batch experiments, 0.5 M NaCl water was blended with NASs, and then water and salt content in the NAS were individually measured. Water absorption efficiencies by NAS 'B' and 'C' were 3.8 and 10.7%, respectively. However, salt rejection efficiency was 98.9% and 58.2%, respectively. NAS 'A' exhibited a higher water absorption efficiency of 35.6%, despite a worse salt rejection efficiency of 24.7%. Molecular dynamic (MD) simulation showed the different interactions of water and salts with each NAS. NAS 'A' formed lattice structured clusters, with the hydrophilic group located outside, and captured a large numbers of water molecules, together with salt ions, inside the cluster pockets. NAS 'B' formed a planar-shaped cluster, where only some water molecules, but no salt ions, migrated to the NAS cluster. NAS 'C', with an ethyl group branch, formed a cluster shaped similarly to that of 'B'; however, the boundary surface of the cluster looked higher than that of 'C', due to the branch structure in solvent. The MD simulation was helpful for understanding the experimental results for water absorption and salt rejection, by demonstrating the various interactions between water molecules and the salts, with the different NAS types.

Spectrophotometric Determination of Chlorpheniramine Maleate with Methyl Orange (메칠오렌지에 의한 말레인산클로르페니라민의 분광광도 정량)

  • Chun, In-Koo
    • Journal of Pharmaceutical Investigation
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    • v.16 no.4
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    • pp.139-147
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    • 1986
  • A singly charged methyl orange(MO) anion was found to be extracted with chlorpheniramine maleate(CPM) as a 1 : 1 complex in chloroform. Of various solvents, MO-chloroform system gave a yellow color for CPM, while in the absence of CPM, an organic phase showed almost no color. In this way, the spectrophotometric method was investigated for the determination of CPM by solvent extraction. The addition of alcoholic bolic acid solution to the solvent extract gave a higher color stability and transparency at least 5 days, but the extract alone lost its color intensity significantly. CPM is determined by measuring the absorbance of the extracts over a range of $1{\sim}7{\times}10^{-4}M\;(39{\sim}273\;{\mu}g/ml)$ in aqueous solution at 423 nm. The molar absorptivity was $2.26{\times}10^3\;l,\;mol^{-1},\;cm^{-1}$. The absorbance of the extract was constant in the range of pH $3.7{\sim}4.6$. This novel method was applied for the determination of CPM in artificial and commercial preparations in comparison with the analytical method of CPM tablets in K.P.IV. The results obtained showed that the former was better in accuracy and time consumption than the latter.

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Graft Copolymerization of Acrylonitrile and 4-Chlorostyrene onto EPDM Rubber. (EPDM 고무에 Acrylonitrile과 4-Chlorostyrene의 그라프트 공중합)

  • Park, Duck-Jei;Ha, Chang-Sik;Lee, Jin-Kook;Cho, Won-Jei
    • Elastomers and Composites
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    • v.24 no.2
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    • pp.110-121
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    • 1989
  • The radical initiated graft copolymerization of acrylonitrile(AN) and 4-chlorostyrene(4-Clst) onto ethylene-propylene-diene terpolymer(EPDM) rubber was investigated under various conditions. Graft copolymer(AU-EPDM-4-Clst) was isolated b: selective solvent extraction and identified by using IR spectroscopy. The percent grafting is determined as a function of solvent, reaction time, and monomer mole ratio. Percent grafting decreased in the order of tetrahydrofuran(THF)>THF/ethyl acetate(EA)(1 : 1)>cyclohexane/EA(1 : 1)>n-hexane/EA(1 : 1). Grafting increased continuously with increasing the reaction time up to 40 hr, beyond which the grafting levelled off. It was observed that percent grafting increased as increasing [4-Clst]/[AN] mole ratio, but decreased when [4-Clst]/[AN] mole ratio was higher than 1.60. The light resistance of graft copolymer(AN-EPDM-4-Clst) was better than that of ABS.

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Versatilities of Calix[4]pyrrole Based Anion Receptors

  • Lee, Chang-Hee
    • Bulletin of the Korean Chemical Society
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    • v.32 no.3
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    • pp.768-778
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    • 2011
  • Calixpyrroles and related macrocycles are non-planer synthetic anion receptors that have attracted considerable attentions in recent years. Although the synthesis of calix[4]pyrrole (known as meso-octamethylporphyrinogen) was reported more than 100 years ago, the anion binding properties were first discovered in 1996. The simple calix[4]pyrroles can be synthesized in single step in high yield by condensation of pyrrole with acetone. The compounds showed preferential binding for halide anions including fluoride, phosphate, carboxylate, and chloride in organic media. Efforts to improve the anion affinity of calix[4]pyrrole and to enhance its selectivity have led to the synthesis of a variety of new calixpyrrole derivatives. Among the various modifications, introduction of straps on one side of the calix[4]pyrroles are the most effective. Incorporation of aromatic rings other than pyrroles also exhibited interesting binding behaviour. Introduction of signalling units as part of the strapping element enable to detect the anions on chromogenic or fluorogenic fashion. Finding of the anion transport properties across the membrane and cytotoxic effects of the calix[4]pyrroles open new window for calixpyrrole-related research. The polymer-incorporated systems have also been employed as anion complexants in solvent-solvent extraction. These old, yet easy-to-make macrocycles have well advanced more recently with the discovery of the ion-pair complexation properties. In this review, the synthetic developments and anion binding properties of calixpyrroles for the last decades will be discussed and will cover the advances in calixpyrrole chemistry.

A Simple and Efficient Method to Determine Montelukast in Rat Plasma Using Liquid-Liquid Extraction and Tandem Mass Spectrometry

  • Kim, Dong Yoon;Lee, Hyo Chun;Jang, Yong Jin;Kim, Jin Hee;Lee, Ha Ryeong;Kang, Myung Joo;Choi, Yong Seok
    • Mass Spectrometry Letters
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    • v.11 no.4
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    • pp.71-76
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    • 2020
  • While montelukast (ML), a cysteinyl-leukotriene type 1 receptor (CysLT1) antagonist is widely used to treat symptoms of rhinitis or asthma, its formulations are mainly limited to solid preparation due to its instability. Recently, there have been attempts to develop various ML dosage forms, and this situation increases the demand of sensitive and creditable methods to determine ML in various samples such as plasma. Thus, here, a simple and efficient method to determine ML in rat plasma using liquid-liquid extraction (LLE) and multiple reaction monitoring was presented. The mixture of DCM:EtOAc (25:75, v/v), the optimized extract solvent for LLE was found to be effective to extract ML without hydrophilic salts and proteins from the sample with limited volume. Also, the use of zafirlukast, instead of expensive ML-d6, as the internal standard makes the present method economical. The developed method was successfully validated in terms of selectivity, matrix effects (-14.8--6.9%), linearity (r230.998 within 0.5-500 ng/mL), sensitivity (the limit of detection and the lower limit of quantitation, ≤0.5 ng/mL), accuracy (88.4-100.6%), precision (3.0-13.3%), and recovery (80.8-86.3%) by following the FDA guidelines. Finally, the applicability of the validated method to pharmacokinetics (PK) studies was confirmed by the successful determination of PK parameters through it following oral administration of Singulair® granule in rats. Therefore, the present method can contribute to the development of new ML formulations through its performance to determine ML in rat plasma efficiently and sensitively.

Acute Toxicity of Emulsifiable Concentrate of Coriander Essential Oils against Cyprinus carpio (고수 정유를 원제로 하는 유제 제형의 잉어에 대한 급성독성)

  • Nam, Tae-Hoon;Jeon, Hwang-Ju;Kim, Kyeongnam;Choi, Yeonseo;Lee, Sung-Eun
    • Korean Journal of Environmental Biology
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    • v.34 no.3
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    • pp.208-211
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    • 2016
  • Essential oils (EOs) extracted from plants possess various biological activities and have been considered as natural insecticides due to their potent insecticidal activities. In regard to develop natural insecticides, EOs are formulated as an emulsifiable concentrate and their acute toxicity against to fishes were determined in a static condition using Cyprinus carpio. Coriander EO was used as an active ingredient mixed with ethanol for solvent and various surface active agents. The tested EOs were obtained from a commercial market, and three different extractions were also undertaken to produce EO using steam distillation, solvent extraction, and supercritical fluid extraction. Among the emulsifiable concentrate including a commercial coriander EO, surface active agents such as Tween 80, sodium dodecyl benzene sulfonate (SDBS), and mixture of SDBS and Nonidet showed acute toxicity to the fish. With the three different EO extraction, coriander EO obtained from supercritical fluids with Triton X-100 exhibited acute toxicity to C. carpio. Taken together, Tetgitol and Nondet are considered as surface active agents for the emulsifiable formulation of coriander EO.

Optimization of Solvent Extraction Process on the Functional Components from Portulaca oleracea Using a Response Surface Methodology (쇠비름의 유용성분 환류추출공정의 최적화)

  • Jo, In-Hee;Kim, Tae-Yeon;Ma, Ji-Bock;Lee, Jin-Ju;Lee, Hyo-Jeong;Choi, Yong-Hee
    • Current Research on Agriculture and Life Sciences
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    • v.29
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    • pp.83-89
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    • 2011
  • Various functional and useful components in Portulaca oleracea were extracted with ethanol and the optimum solvent conditions were set by monitoring of response surface methodology(RSM). A central composite design for optimization was applied to investigate the effects of the three independent variables of extraction temperature, ethanol concentration, and extraction time, on dependent variables including total phenolics, electron-donating ability, brown clolor and total flavonoids of Portulaca oleracea. The content of total phenol was essentially unaffected by extraction time or extraction temperature, but it was highly influenced by ethanol concentration. The maximum total phenol content was 31.70mg/mL obtained at 45.84% of ethanol concentration, $79.66^{\circ}C$, and after 2.67hr of extraction. Electron-donating ability (EDA) was affected by ethanol concentration and the maximum EDA was 74.67mg/mL at 52.95% ethanol concentration, $52.33^{\circ}C$ and 4.84hr of extration time. The browning color was rarely affected by extraction time but, it was highly influenced by ethanol concentration and extraction temperature. The maximum extent of browning color was obtained at 97.75% of ethanol concentraion, $65.88^{\circ}C$ and 2.93hr of extraction time. The content of total flavonoid was significantly influenced by extraction time, and the maximum total flavonoid level was 58.28mg/mL obtained at 96.62% ethanol concentration, $61.87^{\circ}C$ after 3.70hr of extraction. As a result, The optimal conditions for effective extraction were predicted as follows, 70.3% of ethanol concentration, $62.1^{\circ}C$ of extraction temperature and 3.3hr of extraction time.

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Antioxidant and antidiabetic activities of various solvent extracts from Stachys sieboldii Miq. (용매별 초석잠 추출물의 항산화 및 항당뇨 활성)

  • Kang, Jae-Ran;Kang, Min-Jung;Shin, Ji-Hyeon;Park, Ji-Hye;Kim, Dong-il;Chung, Sang-Yong;Shin, Jung-Hye
    • Food Science and Preservation
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    • v.24 no.5
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    • pp.615-622
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    • 2017
  • This study investigated the antioxidant and antidiabetic activities of Stachys sieboldii Miq. extracts by solvents (water, ethanol, butanol, chloroform, and hexane). The contents of total polyphenols (7.18-37.25 mg/g) and flavonoids (0.21-5.21 mg/g) in extracts from Stachys sieboldii Miq. showed a significant difference dependent on the extraction solvents, butanol > ethanol > water > chloroform > hexane. Antioxidant activities by DPPH and ABTS radical scavenging were increased in a dose-dependent manner. These activity trends associated with the extraction solvent were different at each concentration, but resembled phenolic compound contents trend, generally. FRAP value increased in a dose-dependent manner, but there was a difference in radical scavenging activities when comparing between extraction solvents by butanol > ethanol > hexane > chloroform > water on all concentrations. The trend of ${\alpha}$-amylase inhibition of extracts from $1,000{\mu}g/mL$ to $2,000{\mu}g/mL$ was not affected as enzyme activity is promoted and not inhibited. The inhibition of ${\alpha}$-glucosidase was increased in a dose-dependent manner without water extracts, the activity on hexane extracts was higher than others per the extraction solvent. ${\alpha}$-Glucosidase inhibition of hexane extracts showed 57.76% at $250{\mu}g/mL$, which is 2.8 times higher than the second highest chloroform extract (20.65%). From these results, we presume that the active ingredients of Stachys sieboldii Miq. is different according to the extraction solvent and also the activity is different by these major functional groups.