• Title/Summary/Keyword: Liquid-Liquid Extraction

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A Synthesis of Optically Active cis and trans 2-(5-Hydroxypoperidin-2-yl)acetates

  • P.N. Reddy;한상수;정교현
    • Bulletin of the Korean Chemical Society
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    • v.19 no.6
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    • pp.617-618
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    • 1998
  • A simple and reproducible pretreatment method was developed for the determination of dioxins in milk sample. Liquid-liquid extraction (LLE) was used for the initial extraction of the analyte from milk. For the elimination of interferences coextracted from milk, acid treatment followed by multilayer silica gel, and then alumina column clean-up were performed. The clean extract could be obtained without carbon column or high performance liquid chromatographic (HPLC) clean-up procedure. Polychlorinated biphenyles (PCBs) and dioxins were separated on neutral alumina activated at 180 ℃ for 12 hours. The final extract was analyzed by HPLC and high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The recovery of dioxins spiked in milk at 75-300 ppt level was 83.3-98.9% and their relative standard deviation was 4.1-14%.

Analytical Method for Dioxin and Organo-Chlorinated Compounds : (I) Pretreatment of Milk Samples for Dioxin Analysis

  • 양정수;김진영;최용욱;이대운
    • Bulletin of the Korean Chemical Society
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    • v.19 no.6
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    • pp.619-624
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    • 1998
  • A simple and reproducible pretreatment method was developed for the determination of dioxins in milk sample. Liquid-liquid extraction (LLE) was used for the initial extraction of the analyte from milk. For the elimination of interferences coextracted from milk, acid treatment followed by multilayer silica gel, and then alumina column clean-up were performed. The clean extract could be obtained without carbon column or high performance liquid chromatographic (HPLC) clean-up procedure. Polychlorinated biphenyles (PCBS) and dioxins were separated on neutral alumina activated at 180 ℃ for 12 hours. The final extract was analyzed by HPLC and high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The recovery of dioxins spiked in milk at 75-300 ppt level was 83.3-98.9% and their relative standard deviation was 4.1-14%.

Separation of Chromium(VI) Ion in Industrial Waste Water throunh Liquid Surfactant Membrane (산업폐수중 유화액막에 의한 크롬(VI)의 분리)

  • 초민승;강안수;우인성;이영순
    • Journal of the Korean Society of Safety
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    • v.4 no.1
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    • pp.15-24
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    • 1989
  • The transport of Chromium(Vl) ion from waste water throughl the liquid surfactant membrane containing tri-n-octylamine as a carrier, was analyzed by a slab model and was investigated through experiments. For the experiment of membrane stability, concentrations of surfactant and liquid parafnn oil were analyzed. Extraction euperiments were carried out to observe the effect of system variables, such as stirring speed, concentration of carrier, and NaOH in internal aqueous phase, and concentrations of H$_2$SO$_4$and initial chromium(VI) ion in external aqueous phase at $25^{\circ}C$. It is concluded that the most stable formation of liquid membrane emulsion was obtained when surfactant concentration is above 3 wt. % and liquid parafnn oil concentration is 50 vol. %. The transport of chromium(VI) ion in bacth extractor increased with increasing carrier concentration, the volume ratio of emulsion to external aqueous phases, and initial concentration of chromium(VI) ion under the optimum stirring speed of chromium(VI) ion below 2 ppm. The theoretical equation on the transport of chromium(Vl) ion agreed well with the experimental results.

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Analysis of droplet formation under sloshing phenomena in liquid fuel tank (액체 연료 탱크 내 슬로싱 현상에서의 액적 형성 분석)

  • Sungwoo Park;Jinyul Hwang
    • Journal of the Korean Society of Visualization
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    • v.21 no.2
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    • pp.102-110
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    • 2023
  • With the global shift from a carbon-based economy to a hydrogen-based economy, understanding the sloshing phenomenon and its impact on boil-off rate (BOR) in liquid hydrogen (LH2) tank trailers is crucial. Here, we analyze the primary breakup process under sloshing phenomena in a liquid fuel tank. We observe the growth of multiple holes on the sheet-like structures and the formation of ligament structures reminiscent of jet atomization. Through the extraction of three-dimensional liquid regions, we analyze the geometrical characteristics of these regions, enabling the classification of sheets, ligaments, and droplets. The present findings could contribute to understanding the breakup mechanism and hold potential for the development of strategies aimed at minimizing BOR.

Analysis Method of Parabens in Human Breast Milk by LC-MS/MS System (LC-MS/MS 시스템을 이용한 모유 중 파라벤류 분석법 확립)

  • Park, Na-Youn;Lee, Eun-Hee;Kho, Younglim
    • Journal of the Korean Chemical Society
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    • v.60 no.2
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    • pp.118-124
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    • 2016
  • Parabens were commonly used for preventing the growth of microorganisms as preservatives in the pharmaceutical, cosmetic and food industry. Also, parabens are known endocrine disruptors because of their estrogenic effects on human. Parabens affect the endocrine system and show adverse effect such as, genital malformations, precocious puberty and testicular cancer in young children, infants and fetuses. In this study, we developed analytical method for four parabens (methyl paraben, ethyl paraben, propyl paraben, butyl paraben) in human breast milk which frequently consumed by newborn baby. The analytes were extracted using liquid-liquid extraction (LLE) after enzyme hydrolysis with protease and lipase, then quantitative analysis was performed by liquid chromatography tandem mass spectrometry (LC-MS/MS). The method validation results were as follows; the linearity of calibration curves were excellent with coefficient of determinations (r2) higher than 0.999, the limit of detections (LODs) were 0.019~0.044 ng/mL, the accuracies were 85.3~105.9% and the precisions were lower than 10%. The average concentration ± standard deviation of parabens in ten human breast milk sample were MP 0.660 ± 0.519 ng/mL, EP 1.631 ± 2.081 ng/mL and PP 0.326 ± 0.320 ng/mL, and BP was not detected.

Ultrasonic-assisted Micellar Extraction and Cloud-point Pre-concentration of Major Saikosaponins in Radix Bupleuri using High Performance Liquid Chromatography with Evaporative Light Scattering Detection

  • Suh, Joon-Hyuk;Yang, Dong-Hyug;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2637-2642
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    • 2011
  • A new ultrasonic-assisted micellar extraction and cloud-point pre-concentration method was developed for the determination of major saikosaponins, namely saikosaponins -A, -C and -D, in Radix Bupleuri by high performance liquid chromatography with evaporative light scattering detection (HPLC-ELSD). The non-ionic surfactant Genapol X-080 (oligoethylene glycol monoalkyl ether) was chosen as the extraction additive and parameters affecting the extraction efficiency were optimized. The highest yield was obtained with 10% (w/v) Genapol X-080, a liquid/solid ratio of 200:1 (mL/g) and ultrasonic-assisted extraction for 40 min. In addition, the optimum cloud-point pre-concentration was reached with 10% sodium sulfate and equilibration at $60^{\circ}C$ for 30 min. Separation was achieved on an Ascentis Express C18 column (100 ${\times}$ 4.6 mm i.d., 2.7 ${\mu}M$) using a binary mobile phase composed of 0.1% acetic acid and acetonitrile. Saikosaponins were detected by ELSD, which was operated at a $50^{\circ}C$ drift tube temperature and 3.0 bar nebulizer gas ($N_2$) pressure. The water-based solvent modified with Genapol X-080 showed better extraction efficiency compared to that of the conventional solvent methanol. Recovery of saikosaponins ranged from 93.1 to 101.9%. An environmentally-friendly extraction method was successfully applied to extract and enrich major saikosaponins in Radix Bupleuri.

Comparative Study of Extracting Fragrance Allergens by GC-MS/MS

  • Lee, In Ja;Ahn, Jae-Chan;Kim, Bogsoon;Chung, Deukmo
    • Mass Spectrometry Letters
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    • v.8 no.1
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    • pp.18-22
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    • 2017
  • Products containing any one or more of 26 fragrance allergens likely to cause contact allergies, are required under the 2008 domestic cosmetic law to be labeled when their concentrations exceed a certain range. This study focuses on the comparison and development of analytical methods based on headspace-solid phase micro extraction (HS-SPME) and liquid-liquid extraction (LLE) methods followed by GC-MS/MS for 24 of the fragrance allergens excepting for two natural materials in water samples. Using the developed HS-SPME method, 15 of the 24 fragrance allergens were analyzed and 9 compounds which have relatively low $logK_{OW}$ values (below about 2.5) were not extracted, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9969 or more, and the method detection limits (MDL) and the limits of quantification (LOQ) were $0.078{\sim}0.582{\mu}g/L$ and $0.261{\sim}1.940{\mu}g/L$, respectively. In the case of using the optimized LLE method, all 24 fragrance allergens were analyzed, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9957 or more, MDL and LOQ were $0.020{\sim}0.138{\mu}g/L$ and $0.065{\sim}0.440{\mu}g/L$, respectively.

The Effect of Different Particle Size from PAHs Contaminated Sediment by Ultrasonic Irradiation (PAHs로 오염된 침전물의 초음파 처리시 입자크기가 미치는 영향)

  • Na, Seung-Min;Khim, Jee-Hyeong;Cui, Ming-Can;Ahn, Yun-Gyong;Weavers, Linda K.
    • Journal of Environmental Science International
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    • v.19 no.3
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    • pp.379-387
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    • 2010
  • Sediments of Little Scioto (LS) River in Ohio was contaminated by poor disposal of creosote from Baker Wood Creosoting Facility. Among the primary compounds of creosote, Polycyclic Aromatic Hydrocarbons (PAHs) are the most common ingredient PAHs are known for toxic, carcinogenic and mutagenic compounds. There are many difficulties to remove the PAHs in nature environment because their characteristics are having a less water-solubility, volatile and low mobility properties as increasing the molecular weight. The generation of hydroxyl radicals (${\cdot}OH$) and hydrogen peroxide ($H_2O_2$) forms as well as high temperature (5000 K) and pressure (1000 atm) by a physico-chemical effects of ultrasound during a cavitation collapse can promote the degradation and desorption of PAHs in sediment And it can also produces shock wave and microjets which are able to change the size and surface of particle in solid-liquid system as one of physical effects. Therefore, we explored to understand the role of particle size, the effect of elimination for PAHs concentration by ultrasound and optimize the conditions for ultrasonic treatment. The condition of various size of particles (> $150{\mu}m$, < $150{\mu}m$) and solid-liquid ratio (12.5g/L, 25g/L) for the treatment was considered and ultrasonic power (430 W/L) with liquid - hexane extraction and microwave extraction method were applied after ultrasound treatment.

Method development and initial results of testing for perfluorooctane sulfonate (PFOS) and perfluorooctanoic acid (PFOA) in waterproof sunscreens

  • Keawmanee, Sasipin;Boontanon, Suwanna Kitpati;Boontanon, Narin
    • Environmental Engineering Research
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    • v.20 no.2
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    • pp.127-132
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    • 2015
  • Perfluorooctane sulfonate (PFOS) and Perfluorooctanoic acid (PFOA) are persistent environmental pollutants, extremely stable, and possibly adversely affect human health. They are widely used in many industries and consumer goods, including sunscreen products. These substances are stable chemicals made of long carbon chains, having both lipid- and water-repellent qualities. The research objectives are (1) to find the most effective method for the preparation of semi-liquid samples by comparing solid phase extraction (SPE) and centrifugation after Pressurized liquid extraction (PLE), and (2) to determine the contamination levels of PFOS and PFOA in waterproof sunscreen samples. All sunscreen samples were analyzed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Sunscreen samples were purchased from domestic and international brands sold in Thailand. Special chemical properties were considered for the selection of samples, e.g., those found in waterproof, sweat resistant, water resistant, and non-stick products. Considering the factors of physical properties, e.g., operation time, chemical consumption, and recovery percentage for selecting methods to develop, the centrifugation method using 2 mL of extracted sample with the conditions of 12,000 rpm and $5^{\circ}C$ for 1 hour after PLE was chosen. The highest concentrations of PFOS and PFOA were detected at 0.0671 ng/g and 21.0644 ng/g, respectively. Even though present concentrations are found at ng/g levels, the daily use of sunscreen products is normally several grams. Therefore, a risk assessment of PFOS and PFOA contamination in sunscreen products is an important concern, and more attention needs to be paid to the long-term effects on human health.