• Title/Summary/Keyword: Liquid Liquid Extraction

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Quantitative Analysis of Corynomycolic Acids in Fermentation Broth

  • Jang, Ki-Hyo;Park, Yong-Il;Britz, Margaret-L.
    • Journal of Microbiology and Biotechnology
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    • v.12 no.5
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    • pp.793-800
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    • 2002
  • The mycolic acids and fatty acids of mycolic acid- containing bacteria in various types of fluids were analyzed using capillary gas chromatography and mass spectrometry. As model strains, Brevibacterium and Coryebacterium species, which have corynomycolic acids ill the range of $C_{32}C_{36}$ in the whole cell, were investigated. Optimized solvents extraction procedures for the mycolic acids and fatty acids from the culture fluids were: chloroform/methanol (1:2, v/v) as the first extraction solvents fur 4 h; and chlorofunuwater (1:1, v/v) as the second extraction solvents far 1 h. These conditions gave above 95% recovery yields fur mycolic acids from the culture fluids. The mycolic acid profile for the whole cells and the culture fluids were similar fur all the media tested. Thus, the procedure described here could be applied for the identification of mycolic acid-containing bacteria in fermentation broth or liquid from of foods.

Chemical·Structural characterization of lignin extracted from Pitch Pine with Ionic Liquid (1-ethyl-3-methylimidazolium acetate)Pine with Ionic Liquid (1-ethyl-3-methylimidazolium acetate) (이온성액체(1-ethyl-3-methylimidazolium acetate)로 추출한 리기다소나무(pitch pine) 리그닌의 화학·구조 특성)

  • Kim, Jae-Young;Kim, Tae-Seung;Hwang, Hye-Won;Oh, Shin-Young;Choi, Joon-Weon
    • Journal of the Korean Wood Science and Technology
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    • v.40 no.3
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    • pp.194-203
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    • 2012
  • 1-Ethyl-3-methylimidazolium acetate known as efficient biomass pretreatment reagent was used for the extraction of lignin from rigida pine wood (pitch pine), which was called to ionic liquid lignin (ILL), and chemical structural features of ILL were compared with the corresponding milled wood lignin (MWL). The amounts of phenolic hydroxyl groups (Phe-OH) was determined to 10.0% for ILL and 7.2% for MWL, respectively, where those of methoxyl groups (OMe) were 4.9% for ILL and 11.0% for MWL, respectively. The weight average molecular weight (Mw) of ILL (3,995) were determined to ca. 1/2 of that of MWL (8,438) and polydispersity index (PDI: Mw/Mn) suggested that the lignin fragments were more uniform in the ILL (PDI 1.36) than in the MWL (PDI 2.64). The temperature (Tm) corresponding to maximum decomposition rate (Vm) of ILL ($306.6^{\circ}C$) was ca. $35^{\circ}C$ lower than that of MWL ($341.9^{\circ}C$), suggesting that ILL was thermally unstable than MWL, as evidence from the lower Tm for ILL. Moreover, the structural characteristics of ILL and MWL were confirmed by spectroscopic analyses (FT-IR and $^{13}C$-NMR), and these results indicated ionic liquid (1-ethyl-3-methylimidazolium acetate) was chemically or physically bound to ILL.

Characteristics of Tenebrio molitor larvae and Bombyx mori pupae sequentially fermented with Aspergillus oryzae and Bacillus subtilis (Aspergillus oryzae와 Bacillus subtilis를 순차접종 발효한 갈색거저리유충과 누에번데기 발효물의 품질특성)

  • Kang, Sanghun;Chung, Chang-Ho
    • Korean Journal of Food Science and Technology
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    • v.54 no.1
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    • pp.94-102
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    • 2022
  • Defatted soybean, larvae of brown mealworm (Tenebrio molitor), and powdered pupae of silkworm (Bombyx mori) were fermented in solid and liquid forms using Aspergillus oryzae and Bacillus subtilis. The protein degradation rate (NDR) through solid fermentation was the highest in the fermented soybean control sample (54.69±6.54%), followed by silkworm pupae (34.82±5.99%) and brown mealworm larvae (30.54±3.80%). When these edible insects were fermented in liquid form, solid extraction yield was 37.73-46.88%, and protein yield was 47.47-63.02%. NDR of fermented liquid form products increased to 58.90, 52.62, and 50.13% for soybean, brown mealworm larvae, and silkworm pupae, respectively. SDS-PAGE of the liquid fermented products confirmed that microbial fermentation decomposed higher-molecular-weight proteins into small polypeptides. In vitro digestibility of liquid forms of edible insects increased by 1.26 to 1.53 times after fermentation. The protein solubility, foaming ability, and foam stability of liquid-fermented edible insects all tended to increase through fermentation.

A Study on the Hydraulic Characteristics of Rashig Super-Ring Random Packing in a Counter-Current Packed Tower (역류식 충전탑에서 Raschig Super-ring Random Packing의 수력학적 특성에 대한 연구)

  • Kang, Sung Jin;Lim, Dong-Ha
    • Clean Technology
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    • v.26 no.2
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    • pp.102-108
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    • 2020
  • In recent years, packed column has been widely used in separation processes, such as absorption, desorption, distillation, and extraction, in the petrochemical, fine chemistry, and environmental industries. Packed column is used as a contacting facility for gas-liquid and liquid-liquid systems filled with random packed materials in the column. Packed column has various advantages such as low pressure drop, economical efficiency, thermally sensitive liquids, easy repairing restoration, and noxious gas treatment. The performance of a packed column is highly dependent on the maintenance of good gas and liquid distribution throughout a packed bed; thus, this is an important consideration in a design of packed column. In this study, hydraulic pressure drop, hold-up as a function of liquid load, and mass transfer in the air, air/water, and air-NH3/water systems were studied to find the geometrical characteristic for raschig super-ring experiment dry pressure drop. Based on the results, design factors and operating conditions to handle noxious gases were obtained. The dry pressure drop of the random packing raschig super-ring was linearly increased as a function of gas capacity factor with various liquid loads in the Air/Water system. This result is lower than that of 35 mm Pall-ring, which is most commonly used in the industrial field. Also, it can be found that the hydraulic pressure drop of raschig super-ring is consistently increased by gas capacity factor with various liquid loads. When gas capacity factor with various liquid loads is increased from 1.855 to 2.323 kg-1/2 m-1/2 S-1, hydraulic pressure drop increases around 17%. Finally, the liquid hold-up related to packing volume, which is a parameter of specific liquid load depending on gas capacity factor, shows consistent increase by around 3.84 kg-1/2 m-1/2 S-1 of the gas capacity factor. However, liquid hold-up significantly increases above it.

Changes in Flavor Component of Omija, Shizandra Chinensis Baillon, with Various Extraction times (오미자의 용출시간에 따른 풍미성분 변화에 관한 연구)

  • 김유미;김동희;염초애
    • Korean journal of food and cookery science
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    • v.7 no.1
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    • pp.27-34
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    • 1991
  • This study attempted to set up reasonable extraction time of Omija that was put in water for the various components to soak out. Changes of free sugars, organic acids, reducing sugar, total acid and tannin in Omija with various extraction times were investigated (together with the analysis of each components in Omija fruit). 1. High Performance Liquid Chromatography showed fructose, glucose, and sucrose to be the major free sugars of the Omija fruit. Free sugars and reducing sugar value in Omija beverage increased gradually in according with the extraction time, and marked 75.6% per total free sugars and 82.1% per total reducing sugar at 12 hours. 2. Gas Chromatography showed lactic acid, oxalic acid, fumaric acid, levulinic acid, succinic acid, malic acid, citric acid and pyroglutamic acid to be the major organic acids of the Omija fruit. Organic acids and total acids value in Omija beverage increased gradually on proportion to extraction time, and marked 97.0% per total organic acids at 9 hours and 79.0% per total acids at 12 hours. 3. Tannin content in Omija beverage was increased when extraction time was longer but it showed a low percentage as compared with the reducing sugar and total acid. Tannin content marked 48.8% per total tannin at 12 hours. 4. Sensory evaluation revealed that !1 hours of extraction produced the best quality products based in taste, flavor, color and over-all acceptability, considering the data, it seems possible to conclude that the optimum of time for extraction of Omija to water is 9 hours.

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Quantitative analysis of cholesterol in infant formula by isotope dilution liquid chromatography-tandem mass spectrometry (동위원소희석 액체크로마토그래피 질량분석법에 의한 분유 내 콜레스테롤의 정량)

  • Ahn, Eun Jeong;Lee, Hwa Shim;Kim, Byung Joo;Lee, Gae Ho
    • Analytical Science and Technology
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    • v.28 no.6
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    • pp.460-466
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    • 2015
  • An isotope dilution liquid chromatography tandem mass spectrometry was developed as a primary method for the quantitative analysis of cholesterol in infant formula. Cholesterol-d4 was used as an internal standard and spiked into the infant formula sample. In order to release cholesterol out of cholesteryl ester, which is cholesterol bound to fatty acids in infant formula, saponification was carried out. Saponification conditions were optimized with heating temperature, reaction time and the concentration of KOH. The optimum conditions were as follows; heating temperature was 70 ℃, reaction time was 180 min and the concentration of KOH was 0.8 mL of 8 M KOH for about 0.1 g infant formula sample. Extraction of cholesterol out of sample solution was carried out with hexane uisng liquid-liquid extraction. Chromatographic analysis was carried out using Phenomenex Kinetex C18 column. Mobile phase was 0.1% acetic acid in methanol/water (v/v, 99/1) and flow rate was 0.3 mL/min. Cholesterol and cholesterol-d4 were monitored at mass transfer m/z 369/259 and 373/263 respectively. Reproducibility of the method was evaluated to be 0.23% of the measurement result. The expanded uncertainty of the measurement result of cholesterol in infant formula was approximately 1.9% at a 95% confidence level. NIST standard reference material having certified values of cholesterol in infant formula, was analyzed in order to verify this method. The ID-LC/MS/MS results were well agreed with the certified values of NIST SRM within the uncertainty.

Separation and Elution Behaviors of Some Metal-2-hydroxyarylazopyrazolone Chelates by Reversed Phase High Performance Liquid Chromatography (I) (역상 액체 크로마토그래피에 의한 금속-2-hydroxyarylazopyrazolone 유도체 킬레이트의 용리거동 및 동시분리에 관한 연구 (I))

  • Lee, Chang-Heon;Kang, Chang-Hee;Kim, Eun-Kyung;Lee, Won
    • Analytical Science and Technology
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    • v.7 no.1
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    • pp.103-114
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    • 1994
  • The elution behaviors of Ni(II), Cu(II), Co(II), and Cr(II) in 1-phenyl-3-methyl-4(2-hydroxy-5-X-phenylazo)-5-pyrazolone, [Pm(2-OH)(5-X)PaPz](X=H, $CH_3$, $NO_2$, Cl) chelates have been studied by reversed phase HPLC. Thirteen metal-[Pm(2-OH)(5-X)PaPz] chelates were prepared and characterized by UV, IR, MS, and ICP spectroscopic methods. These metal-2-hydroxyarylazopyrazolone chelates were successfully separated on Novapak-$C_{18}$ column using methanol/water mixtures as a mobile phases. It was found that the chelates were eluted properly in an acceptable range of the capacity factor value($0{\leq}log\;k^{\prime}{\leq}1$). The dependence of the capacity factor(log k') on the volume fraction of water in the binary mobile phase showed a good linearity. Also, there was a good linear dependence of the capacity factor on the liquid-liquid extraction distribution ratio($D_c$) in methanol-water/n-pentadecane extraction system by the batch method. It suggested that the retention of the chelates in the reverse phase liquid chromatographic system be largely due to the solvophobic effect.

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A Study on the Elution Mechanism of Ni(II)-Isonitrosoethylacetoacetate Imine Chelates by Reversed Phase High Performance Liquid Chromatography (역상 액체 크로마토그래피에 의한 Ni(II)-Isonitrosoethylacetoacetate Imine 유도체 킬레이트의 용리 메카니즘에 관한 연구)

  • Kim In-Whan;Choi Gang-Yeol;Lee Man-Ho;Kang Chang-Hee;Lee, Won
    • Journal of the Korean Chemical Society
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    • v.36 no.5
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    • pp.697-708
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    • 1992
  • Liquid Chromatographic behavior of Ni(II) in Isonitrosoethylacetoacetate Imine(IEAA-NR), Ni(IEAA-NH)(IEAA-NR)(R = H, CH_3, C-2H_5, n-C_4H_9, C_6H_5-CH_2) chelates were investigated by reversed-phase HPLC on Micropak MCH-5 column using methanol/water as mobile phase. The optimum conditions for the separation of Ni(IEAA-NH)(IEAA-NR) chelates were examined with respect to the effect of the flow rate, sample solvent, mobile phase strength and column temperature. It was fo$und that metal chelates were properly eluted in an acceptable range of capacity factor value(0{\le}logk'{\le}1). The dependence of the logarithm of capacity factor (k') on the volume fraction of water in the binary mobile phase as well as on the liquid-liquid extraction distribution ratio (Dc) in methanol-water/n-alkane extraction system showed the good linearties, and the dependence of the logarithm of capacity factor (k') on the column temperature and on the enthalpy exhibited the good linearties, and the compensation temperature ({\beta}) from the slope was 773.47{\circ}K. It was suggested that the retention of metal chelates was largely affected by the hydrophobic effect.

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Simultaneous determination of carbaryl & organophosphorous pesticides in water by liquid chromatography-tandem mass spectrometry (LC/MS/MS를 이용한 수중의 카바릴·유기인계 농약 동시분석)

  • Park, Keun-Young;Shin, Jung-Chul;Pyo, Dongjin
    • Analytical Science and Technology
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    • v.31 no.1
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    • pp.39-46
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    • 2018
  • Carbaryl and seven organophosphorous pesticides were analyzed simultaneously using on-line solid phase extraction (on-line SPE) coupled with liquid chromatography tandem mass spectrometry (LC/MS/MS). The target pesticides are Carbaryl, Methyl demeton, Fenitrothion, Malathion, Parathion, Phenthoate, Diazinon, and EPN. This method includes the direct injection of $500{\mu}L$ in the water sample, a 15 min separation period using a rapid resolution liquid chromatography system with on-line SPE, and detection through electrospray ionization (ESI) positive mode. The percentage of recovery of all pesticides ranged from 85.3 % to 100 %. This method showed an accuracy of ${\geq}90.0%$, possessing limits of detection and quantification within 0.05 to $0.28{\mu}g/L$ and 0.16 to $0.89{\mu}g/L$, respectively. The correlation coefficients (r) for the calibration curves within a range of 0.5 to $8.0{\mu}g/L$ were higher than 0.99. The evaluation results showed the efficacy of the method for all contents, and no pesticides were detected in the water quality sample.

Separation and Elution Behavior of Some Iron(Ⅲ)porphyrin Complexes by Reversed-Phase Liquid Chromatography (역상 액체 크로마토그래피에 의한 Iron(Ⅲ)porphyrin 착화합물들의 분리 및 용리거동에 관한 연구)

  • Chang Hee Kang;In Whan Kim;Won Lee
    • Journal of the Korean Chemical Society
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    • v.37 no.12
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    • pp.1035-1046
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    • 1993
  • Some iron(III)porphyrin complexes were prepared, and identified by the spectroscopic methods. Elution behavior of iron(III)porphyrin complexes was investigated by reversed-phase HPLC. The optimum conditions for the separation of iron(III)porphyrin complexes were examined with respect to flow rate and mobile phase strength. These complexes were successfully separated on NOVA-PAK $C_{18}$ column using methanol / water(95/5) for $[T_pCF_3PP)Fe(R)]$ and methanol / water (98/2) for $[(P)Fe(C_6F_5)]$ as a mobile phase. It was found that these complexes were largely eluted in an acceptable range of capacity factor value ($0{\leq}logk'{\leq}1$). The dependence of the capacity factor (k') on the volume fraction of water in the binary mobile phase as well as the dependence of k' on the liquid-liquid extraction distribution ratio$(D_c)$ in methanol-water / n-pentadecane extraction system showed a good linearity. It means that the retention of iron(III)porphyrin complexes on NOVA-PAK $C_{18}$ column is largely due to the solvophobic effect. Also, there was a good linear dependence of the capacity factor(k') on the column temperature and enthalpy calculated by van't Hoff plot. From these results, it was confirmed that the retention mechanism of iron(III)porphyrin complexes in reversed-phase liquid chromatography was invariant under the condition of various temperature, and the solvophobic binding process exhibited isoequilibrium behavior.

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