• Title/Summary/Keyword: Liquid Liquid Extraction

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Integration of Headspace Solid Phase Micro-Extraction with Gas Chromatography for Quantitative Analysis of Formaldehyde

  • Lo, Kong Mun;Yung, Yen Li
    • Bulletin of the Korean Chemical Society
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    • v.34 no.1
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    • pp.139-142
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    • 2013
  • A study was carried out to evaluate the solid phase micro-extraction (SPME) for formaldehyde emission analysis of uncoated plywood. In SPME, formaldehyde was on-fiber derivatized through headspace extraction and analyzed by gas chromatography coupled with mass spectrometry (GC/MS). The SPME was compared with desiccators (DC-JAS 233), small-scale chamber (SSC-ASTM D6007) and liquid-liquid extraction (LLE-EPA 556) methods which were performed in accordance with their respective standards. Compared to SSC (RSD 4.3%) and LLE (RSD 5.0%), the SPME method showed better repeatability (RSD 1.8%) and not much difference from DC (RSD 1.4%). The SPME has proven to be highly precise (at 95% confidence level) with better recovery (REC 102%). Validation of the SPME method for formaldehyde quantitative analysis was evidenced. In addition, the SPME by air sampling directly from plywood specimens (SPME-W) correlated best with DC ($r^2$ = 0.983), followed by LLE ($r^2$ = 0.950) and SSC ($r^2$ = 0.935).

Headspace Hanging Drop Liquid Phase Microextraction and GC-MS for the Determination of Linalool from Evening Primrose Flowers

  • Kim, Nam-Sun;Jung, Mi-Jin;Yoo, Zoo-Won;Lee, Sun-Neo;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.26 no.12
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    • pp.1996-2000
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    • 2005
  • Headspace hanging drop liquid phase micro-extraction (HS-HD-LPME) is studied as a novel solvent-based sample pretreatment method for floral volatile aroma compounds. This paper reports on application of the HSHD- LPME combined with GC-MS for the analysis of linalool component emitted from evening primrose flowers. The effect of several variables on the method performance was investigated. Additionally, the separation of enantiomers on a cyclodextrin capillary column was performed to identify chirality of (−)-linalool component. Since the unsurpassed volume of a few micro-liters of solvent is used, there is minimal waste or exposure to toxic organic solvents. This method enables to combine extraction, enrichment, clean-up, and sample introduction into a single step prior to the chromatographic process.

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.