• Title/Summary/Keyword: Liquid-Liquid Extraction

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Simultaneous determination of saikosaponin derivatives in Bupleurum falcatum by HPLC-ELSD analysis using different extraction methods

  • Choi, Jungwon;Kim, Juree;Kang, Sam Sik;Lee, Sanghyun
    • Journal of Applied Biological Chemistry
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    • v.64 no.1
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    • pp.57-61
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    • 2021
  • Saikosaponin derivatives such as saikosaponins A, B1, B2, B3, B4, C, and D present in Bupleurum falcatum were analyzed by a high performance liquid chromatograph equipped with an evaporative light scattering detector, using different extraction solvents (water and 70% ethanol). The samples were injected into a YMC Pack Pro C18 column and separated using a gradient elution system with a mobile phase composed of acetonitrile and water at a flow rate of 1.1 mL/min. The content of saikosaponin derivatives was higher in 70% ethanol extract than in water extract. This study provides an efficient analytical method for determining the optimal conditions for extraction of saikosaponin derivatives, which can be used as a basis for development of functional foods and pharmaceutical products from B. falcatum.

Determination of Non-Steroidal Anti-Inflammatory Drugs in Human Urine Sample using HPLC/UV and Three Phase Hollow Fiber-Liquid Phase Microextraction (HF-LPME)

  • Cha, Yong Byoung;Myung, Seung-Woon
    • Bulletin of the Korean Chemical Society
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    • v.34 no.11
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    • pp.3444-3450
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    • 2013
  • Three phase hollow fiber-liquid phase microextraction (HF-LPME), which is faster, simpler and uses a more environmentally friendly sample-preparation technique, was developed for the analysis of Non-Steroidal Anti-Inflammatory Drugs (NSAIDs) in human urine. For the effective simultaneous extraction/concentration of NSAIDs by three phase HF-LPME, parameters (such as extraction organic solvent, pH of donor/acceptor phase, stirring speed, salting-out effect, sample temperature, and extraction time) which influence the extraction efficiency were optimized. NSAIDs were extracted and concentrated from 4 mL of aqueous solution at pH 3 (donor phase) into dihexyl ether immobilized in the wall pores of a porous hollow fiber, and then extracted into the acceptor phase at pH 13 located in the lumen of the hollow fiber. After the extraction, 5 ${\mu}L$ of the acceptor phase was directly injected into the HPLC/UV system. Simultaneous chromatographic separation of seven NSAIDs was achieved on an Eclipse XDB-C18 (4.6 mm i.d. ${\times}$ 150 mm length, 5 ${\mu}m$ particle size) column using isocratic elution with 0.1% formic acid and methanol (30:70) at a HPLC-UV/Vis system. Under optimized conditions (extraction solvent, dihexyl ether; $pH_{donor}$, 3; $pH_{acceptor}$, 13; stirring speed, 1500 rpm; NaCl salt, 10%; sample temperature, $60^{\circ}C$; and extraction time, 45 min), enrichment factors (EF) were between 59 and 260. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of 5-15 ng/mL and 15-45 ng/mL, respectively. The relative recovery and precision obtained were between 58 and 136% and below 15.7% RSD, respectively. The calibration curve was linear within the range of 0.015-0.96 ng/mL with the square of the correlation coefficient being more than 0.997. The established method can be used to analyse of NSAIDs of low concentration (ng/mL) in urine.

Inclusion Extraction of Alkali Metals by Emulsion Liquid Membranes and Nano-baskets of p-tert-Calix[4]arene Bearing Di-[N-(X)sulfonyl Carboxamide] and Di-(1-propoxy) in ortho-cone Conformation

  • Mokhtari, Bahram;Pourabdollah, Kobra
    • Bulletin of the Korean Chemical Society
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    • v.33 no.5
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    • pp.1509-1516
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    • 2012
  • Nano-assisted inclusion separation of alkali metals from basic solutions was reported by inclusion-facilitated emulsion liquid membrane process. The novelty of this study is application of nano-baskets of calixarene in the selective and efficient separation of alkali metals as both the carrier and the surfactant. For this aim, four derivatives of $p-tert-calix$[4]arene bearing different sulfonamide moieties were synthesized and their inclusion-extraction parameters were optimized including the calixarene scaffold $\mathbf{3}$ (4 wt %) as the carrier/demulsifier, the commercial kerosene as diluent in membrane, sulphonic acid (0.2 M) and ammonium carbonate (0.4 M) as the strip and the feed phases, the phase and the treat ratios of 0.8 and 0.3, mixing speed (300 rpm), and initial solute concentration (100 mg/L). The selectivity of membrane over more than ten interfering cations was examined and the results reveled that under the optimized operating condition, the degree of inclusion-extraction of alkali metals was as high as 98-99%.

Headspace Hanging Drop Liquid Phase Microextraction and Gas Chromatography-Mass Spectrometry for the Analysis of Flavors from Clove Buds

  • Jung, Mi-Jin;Shin, Yeon-Jae;Oh, Se-Yeon;Kim, Nam-Sun;Kim, Kun;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.27 no.2
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    • pp.231-236
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    • 2006
  • A novel sample pretreatment technique, headspace hanging drop liquid phase microextraction (HS-LPME) was studied and applied to the determination of flavors from solid clove buds by gas chromatography-mass spectrometry (GC-MS). Several parameters affecting on HS-LPME such as organic solvent drop volume, extraction time, extraction temperature and phase ratio were investigated. 1-Octanol was selected as the extracting solvent, drop size was fixed to 0.6 $\mu$L. 60 min extraction time at 25 ${^{\circ}C}$ was chosen. HS-LPME has the good efficiency demonstrated by the higher partition equilibrium constant ($K_{lh}$) values and concentration factor (CF) values. The limits of detection (LOD) were 1.5-3.2 ng. The amounts of eugenol, $\beta$-caryophyllene and eugenol acetate from the clove bud sample were 1.90 mg/g, 1.47 mg/g and 7.0 mg/g, respectively. This hanging drop based method is a simple, fast and easy sample enrichment technique using minimal solvent. HSLPME is an alternative sample preparation method for the analysis of volatile aroma compounds by GC-MS.

Polymer Dispersed Liquid Crystal for Enhanced Light Out-Coupling Efficiency of Organic Light Emitting Diodes

  • Gasonoo, Akpeko;Ahn, Hyeon-Sik;Lee, Jonghee;Kim, Min-Hoi;Lee, Jae-Hyun;Choi, Yoonseuk
    • Journal of IKEEE
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    • v.24 no.1
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    • pp.140-146
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    • 2020
  • We investigated light extraction film based on polymer dispersed liquid crystal (PDLC) for application in organic light emitting diodes (OLEDs). At least 30 seconds of direct UV irradiation process for curing PDLC film on a bottom-emitting OLEDs was successfully achieved without damage on the intrinsic properties of the OLED. We demonstrated that high haze and transmittance can be tuned simultaneously by controlling the UV curing time. By adding PDLC as an external layer without any additional treatment, the light scattering and extraction is increased. Consequently, a PDLC scattering film with 89.8% and 59.9 of total transmittance and haze respectively, achieved about 16% of light intensity enhancement from integrating sphere measurement.

Development of Sensitive Analytical Method of Rhodanthpyrone A by a LC-MS/MS and its Application to Bioavailability Study in Rats

  • Kang, Bitna;Yoon, Jeong A;Song, Im-Sook;Han, Young Taek;Choi, Min-Koo
    • Mass Spectrometry Letters
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    • v.10 no.3
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    • pp.88-92
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    • 2019
  • A sensitive analytical method of rhodanthpyrone A in rat plasma was developed using a liquid chromatography-tandem mass spectrometry (LC-MS/MS). Rhodanthpyrone A and rhodanthpyrone B (internal standard) in rat plasma were extracted by a liquid-liquid extraction method with ethyl acetate. This extraction method gave results in high and reproducible extraction recovery in the range of 73.75-79.90% with no interfering peaks around the peak elution time of rhodanthpyrone A and B. The standard calibration curves for rhodanthpyrone A ranged from 0.5 to 2000 ng/mL were linear with $r^2$ > 0.994 and the inter- and intra-day accuracy and precision and the stability were within acceptance criteria. Using this validated analytical method, pharmacokinetics of rhodanthpyrone A following intravenous and oral administration of rhodanthpyrone A at doses of 2 mg/kg and 30 mg/kg, respectively, were investigated. Rhodanthpyrone A in rat plasma showed multi-exponential elimination pattern with high clearance and volume of distribution values. The absolute oral bioavailability of this compound was calculated as 3.7%. Collectively, the newly developed sensitive LC-MS/MS analytical method of rhodanthpyrone A could be successfully applied to investigate the pharmacokinetic properties of this compound and would be useful for the further studies on the efficacy, toxicity, and biopharmaceutics of rhodanthpyrone A.

Analysis of trace odorous compounds (geosmin and 2-methylisoborneol) in water by using GC/MS (물 중의 극미량 냄새 유발 물질인 Geosmin과 2-methylisoborneol의 GC/MS 분석법 연구)

  • Kim, Tae-Jon;Kim, Byung-Joo;So, Hun-Young;Kwang, Ho
    • Analytical Science and Technology
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    • v.15 no.6
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    • pp.534-539
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    • 2002
  • We established an analytical method for the measurement of trace amounts of earthy/musty odorous geosmin (GSM) and 2-methylisoborneol (2-MIB) in water using GC/MS. Water samples were extracted with n-hexane (liquid-liquid extraction, LLE) and the extracts were measured by GC/MS. The extraction yields of the two compounds were tested to be ($87{\pm}8$)% and ($78{\pm}8$)%, respectively. The limits of quantitation (LOQs) of the two compounds by this method were greatly improved to ~0.3 ng/L. The analytical methods were applied to analyze water samples from several rivers in Korea and waters after water treatment processes. The highest levels of geosmin and 2-methylisoborneol in raw water from a river were measured to be ($4.2{\pm}0.4$) ng/L and ($44{\pm}4$) ng/L, respectively. The levels only slightly decreased to ($1.3{\pm}0.1$) ng/L and ($18{\pm}2$) ng/L even after water treatment, indicating that the odorous compounds were not properly removed by the treatment processes.

Phytochemical analysis of Panax species: a review

  • Yang, Yuangui;Ju, Zhengcai;Yang, Yingbo;Zhang, Yanhai;Yang, Li;Wang, Zhengtao
    • Journal of Ginseng Research
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    • v.45 no.1
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    • pp.1-21
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    • 2021
  • Panax species have gained numerous attentions because of their various biological effects on cardiovascular, kidney, reproductive diseases known for a long time. Recently, advanced analytical methods including thin layer chromatography, high-performance thin layer chromatography, gas chromatography, high-performance liquid chromatography, ultra-high performance liquid chromatography with tandem ultraviolet, diode array detector, evaporative light scattering detector, and mass detector, two-dimensional high-performance liquid chromatography, high speed counter-current chromatography, high speed centrifugal partition chromatography, micellar electrokinetic chromatography, high-performance anion-exchange chromatography, ambient ionization mass spectrometry, molecularly imprinted polymer, enzyme immunoassay, 1H-NMR, and infrared spectroscopy have been used to identify and evaluate chemical constituents in Panax species. Moreover, Soxhlet extraction, heat reflux extraction, ultrasonic extraction, solid phase extraction, microwave-assisted extraction, pressurized liquid extraction, enzyme-assisted extraction, acceleration solvent extraction, matrix solid phase dispersion extraction, and pulsed electric field are discussed. In this review, a total of 219 articles published from 1980 to 2018 are investigated. Panax species including P. notoginseng, P. quinquefolius, sand P. ginseng in the raw and processed forms from different parts, geographical origins, and growing times are studied. Furthermore, the potential biomarkers are screened through the previous articles. It is expected that the review can provide a fundamental for further studies.

Determination of itraconazole in human plasma by high performance liquid chromatography (HPLC/UV를 이용한 혈장 중 이트라코나졸의 분석)

  • Jang, Hae Jong;Lee, Ye Rie;Lee, Kyung Ryul;Han, Sang-Beom;Kang, Seung Woo;Lee, Hee Joo
    • Analytical Science and Technology
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    • v.19 no.3
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    • pp.239-243
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    • 2006
  • This method is used for the determination of itraconazole in human plasma by liquid-liquid extraction and high performance liquid chromatography. Felodipine was used as an internal standard. After extraction of the plasma with diethyl ether, the centrifuged upper layer was then transferred. The supernantant was evaporated and then reconsituted with mobile phase. The mobile phase was composed of 10 mM ammonium acetate adjusted to pH 7 by phosphoric acid with a flow rate of 0.2 mL/min. A C18 reversed-phase column with a pre-column was used as the analytial column. Linear detection responses were obtained for itraconzole concentration range for 2~1,000 ng/mL. The correlation coefficient of linear regression($R^2$) was 0.9991, limit of quantification (LOQ) was 2 ng/mL, reproducibility was less than 10.8 %, and accuracy was 97.2~108.2%. This method has been successfully applied to the pharmacokinetic study of itraconazole in human plasma.

Extraction Methods for Recovering Malachite Green and Leucomalachite Green (추출방법들에 의한 Malachite Green과 Leucomalachite Green 회수율)

  • Bae, Jin-Han;Yun, Young-Soo;Yoon, Sung-Ho;Choi, Kwang-Jin;Lee, Jeong-Seon;Lim, Chi-Won;Kim, Yeon-Kye;Park, Hee-Yeon
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.41 no.1
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    • pp.13-19
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    • 2008
  • Malachite green (MG), a triphenylmethane dye, is carcinogenic, mutagenic, teratogenic, a respiratory toxin, and causes chromosomal fractures. It is not permitted for use as an aquaculture veterinary drug in a number of countries. Sensitive extraction methods for MG and leucomalachite green (LMG), which have long residence times in fish tissues, were developed. For LMG, the average recovery of liquid extraction (LE) ranged from 41.71 (yellowtail) to 71.60% (snakehead); the recovery of liquid-liquid extraction (LLE) was between 67.68 (yellowtail) and 83.68% (snakehead); and the average recovery of solid-phase extraction (SPE) ranged from 84.16 (yellowtail) to 92.92% (shrimp). The recovery of MG was less than 30% with SPE. However, the dye is found primarily as the colorless reduced leuco form in fish tissues.