• 제목/요약/키워드: Liquid-Liquid Extraction

검색결과 1,074건 처리시간 0.032초

하수처리시설 고상시료 중 잔류의약물질 분석을 위한 전처리법 평가 및 적용 (Evaluation and application of pretreatment methods for pharmaceuticals and personal care products in the solid phase of sewage samples)

  • 박준원;김창수;주병규;이원석;정현미;정동환
    • 상하수도학회지
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    • 제32권6호
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    • pp.559-572
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    • 2018
  • The aim of this study was to evaluate pretreatment methods for 27 pharmaceuticals and personal care products (PPCPs) in various sewage samples using a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) and online solid-phase extraction with LC-MS/MS. Extraction efficiencies of PPCPs in the solid phase under different experimental conditions were evaluated, showing that the highest recoveries were obtained with the addition of sodium sulfate and ethylenediaminetetraacetic acid disodium salt dehydrate in acidified conditions. The recoveries of target compounds ranged from 91 to 117.2% for liquid samples and from 61.3 to 137.2% for solid samples, with a good precision. The methods under development were applied to sewage samples collected in two sewage treatment plants (STPs) to determine PPCPs in liquid and solid phases. Out of 27 PPCPs, more than 19 compounds were detected in liquid samples (i.e., influent and effluent) of two STPs, with concentration ranges of LOQ-33,152 ng/L in influents and LOQ-4,523 ng/L in effluents, respectively. In addition, some PPCPs such as acetylsalicylic acid, ibuprofen, and ofloxacin were detected at high concentrations in activated sludge as well as in excess sludge. This methodology was successfully applied to sewage samples for the determination of the target compounds in STPs.

고속액체 크로마토크래피에 의한 커피, 홍차, 녹차중의 카페인 정량에 관한 연구 (A Study on the Determination of Caffeine in Coffee, Black tea and Green Tea by high performance Liquid Chromatography)

  • 권익부;이윤수;우상규;이충영;서준걸
    • 한국식품위생안전성학회지
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    • 제5권4호
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    • pp.213-217
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    • 1990
  • 커피, 홍차, 녹차중의 카페인 함량을 간단하고 신속하게 정량하는 방법을 검토하였다. 역상계 액체크로마토그래피에 의한 카페인 정량은 메타놀-초산-물(20 : 1 : 79)을 이동상으로 하여 ${\mu}-Bondapak$ C18 컬럼하에서 이루어졌다. 카페인의 검출에는 UV검출기를 사용하여 280 mm에서 행하였다. Sep-Pak alumina A 카트리지를 이용한 간단한 전처리를 통해 효과적으로 카페인의 추출 및 clean-up를 행하였다. 카페인의 첨가 회수율은 95.2~101.3%이었고 분석의 재현성은 상대표준 편차로서 0.10~0.62%이었으며 검출한계는 $0.1;\mu\textrm{g}$/ml이었다.

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Reactive separation of boron using a liquid membrane of diol in vegetable oil

  • Hossain, Md. M.;Maraqa, M.A.
    • Membrane and Water Treatment
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    • 제8권1호
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    • pp.19-34
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    • 2017
  • Boron exists in dilute concentrations in sea water, ground water and waste waters. Reactive liquid extraction can be used for removing boron to make the treated water suitable for drinking and irrigation, with its final concentration less than 0.5 ppm. The results of equilibrium experiments are reported on the removal of boron using 2-butyl-2-ethyl-1, 3-propanediol (BEPD as a nonionic carrier) in sunflower oil, a non-traditional solvent. The results of removal of boron from aqueous solutions in the concentration range 0.5-20 ppm are presented. It is shown that this new liquid membrane system, is able to remove boron from ground waters at their natural pH of 6-8 (without any chemical addition for pH adjustments). The removal efficiency is good when the process is upgraded to a hollow-fibre membrane contactor and approximately 45% boron can be removed in a single-stage contact. There are additional advantages of this new approach that includes reduced operational health and safety and environmental issues. The results reported here provide guidelines to the development of boron removal process using renewable, biodegradable, safe and cheap solvent system such as sunflower oil.

유기산의 분리를 위한 유화액막의 수학적 모델 (Modeling of Liquid Emulsion Membrane for Organic Acid Separation)

  • Mok, Young Sun;Lee, Won Kook
    • 멤브레인
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    • 제5권1호
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    • pp.44-57
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    • 1995
  • 내부산의 탈거제로 탄산나트륨을 함유하는 유화액막의 거동을 묘사하기 위하여 수학적 모델이 제시되었다. 젖산의 회분식 추출 실험 결과가 모델의 계산 결과와 비교되었는데, 모델의 계산 결과는 담체농도, 탈거제농도, 교반속도, 처리비와 같은 변수의 영향을 잘 예측할 수 있었다. 유화액막의 주요 문제 중의 하나인 에멀젼의 팽윤을 줄이기 위하여, 액체 파라핀, n-데칸올, 사이클로헥사논, 스판-85 같은 막 첨가제가 사용되었다. 사용된 모든 첨가제는 팽윤 정도를 줄이는데 어느 정도 효과가 있었다. 사이클로헥사논은 팽윤을 줄일 뿐만 아니라, 젖산의 전달 속도를 크게 증가시키는 것으로 관찰되었다.

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Simultaneous Determination of the Novel Neuroprotective Agent KR-31378 and its Metabolite KR-31612 Using High Performance Liquid Chromatography with Tandem Mass Spectrometry in Human Plasma

  • Kim, John;Ji, Hye-Young;Yoo, Sung-Eun;Kim, Sun-Ok;Lee, Dong-Ha;Lim, Hong;Lee, Hye-Suk
    • Archives of Pharmacal Research
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    • 제25권5호
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    • pp.647-651
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    • 2002
  • An LC/MS/MS method for the simultaneous determination of a neuroprotective agent for ischemia-reperfusion damage, KR-31378 and its N-acetyl metabolite KR-31612 in human plasma was developed. KR-31378, KR-31612 and the internal standard. KR-31543 were extracted from human plasma by liquid-liquid extraction. A reverse-phase HPLC separation was performed on Luna phenylhexyl column with the mixture of acetonitrile-5 mM ammonium formate (55:45, v/v) as mobile phase. The detection of analytes was performed using an electrospray ionization tandem mass spectrometry in the multiple reaction monitoring mode. The lower limits of quantification for KR-31378 and KR-31612 were 2.0 ng/ml. The method showed a satisfactory sensitivity, precision, accuracy, recovery and selectivity.

Accurate Determination of Malachite Green and Leucomalachite Green in Fish using Isotope Dilution Liquid Chromatography/Mass Spectrometry (ID-LC/MS)

  • Ahn, Seong-Hee;Kim, Byung-Joo;Lee, Yun-Jung;Kim, Jeong-Kwon
    • Bulletin of the Korean Chemical Society
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    • 제31권11호
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    • pp.3228-3232
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    • 2010
  • Malachite green (MG) has been used world-widely in aquaculture as a parasiticide or fungicide. Although MG performed successfully, it has not been permitted for use in aquaculture from European Union, USA, and Canada because of its carcinogenicity and mutagenicity. We developed a sensitive and specific method to determine MG and its principal metabolite, leucomalachite green (LMG), respectively by isotope dilution liquid chromatography mass spectrometry (ID-LC/MS). To enhance the extraction recovery of MG and LMG from fish tissue, an additional step, saponification, was introduced in sample preparation process to remove fat in sample extract, which hampered the performance of SPE columns. The residue of MG and LMG in fish was analyzed using liquid chromatography mass spectrometry in the selected ion monitoring (SIM) mode by monitoring at m/z 329 and 334 for MG and $d_5$-MG and at m/z 331 and 337 for LMG and $^{13}C_6$-LMG, respectively. This method was validated by comparing with the value of the reference material provided by Laboratory Government Chemistry (LGC). The results agreed within the measurement uncertainty and the accuracy was much improved than the provided reference value by LGC.

LC/MS/MS를 이용한 원숭이 혈액에서의 Doxifluridine과 대사체 5-FU 동시분석법 개발 및 Validation (Quantitative Determination of Doxifluridine and 5-FU in Monkey Serum Using LC/MS/MS)

  • 우영아;김기환;김원;이종화;정은주;김진호;박귀례;김충용
    • 약학회지
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    • 제51권3호
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    • pp.174-178
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    • 2007
  • A reverse-phase high performance liquid chromatography method with electrospray ionization and detection by mass spectrometry is described for the simultaneous determination of doxifluridine and its active metabolite 5-flu-orouracil (5-FU) in monkey serum. The method has greater sensitivity and simpler process than previous published methods with good accuracy and precision. A proper liquid/liquid extraction was used to extract simultaneously doxifluridine and 5-FU which has considerable difference in the polarity. Extracts were analyzed using LC/MS/MS providing a short analysis time within 5 min. The lower limit of quantification was validated at 10.0 ng/ml of serum for both doxifluridine and 5-FU. Accuracy and precision of quality control (QC) samples for both analytes met FDA Guidance criteria of ±15% for average QC accuracy with coefficients of variation less than 15%. The method will be applicable for preclinical studies and bioequivalence studies.

Simultaneous Determination of Cysteamine and Cystamine in Cosmetics by Ion-Pairing Reversed-Phase High-Performance Liquid Chromatography

  • Kim, Yejin;Na, Dong Hee
    • Toxicological Research
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    • 제35권2호
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    • pp.161-165
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    • 2019
  • Cysteamine has been used in cosmetics as an antioxidant, a hair straightening agent, and a hair waving agent. However, recent studies indicate that cysteamine can act as an allergen to hairdressers. The objective of this study was to develop and validate a simple and effective reversed-phase high-performance liquid chromatography (RP-HPLC) method for the measurement of cysteamine and its dimer, cystamine. Sodium 1-heptanesulfonate (NaHpSO) was used as an ion-pairing agent to improve chromatographic performance. Separation was performed on a Gemini C18 column ($250mm{\times}4.6mm$, $5{\mu}m$ particle size) using a mobile phase composed of 85:15 (v/v) 4 mM NaHpSO in 0.1% phosphoric acid:acetonitrile. UV absorbance was monitored at 215 nm. The RP-HPLC method developed in this study was validated for specificity, linearity, limit of detection, limit of quantitation, precision, accuracy, and recovery. Cysteamine and cystamine were chromatographically resolved from other reducing agents such as thioglycolic acid and cysteine. Extraction using water and chloroform resulted in the recovery for cysteamine and cystamine ranging from 100.2-102.7% and 90.6-98.7%, respectively. This validated RP-HPLC method would be useful for quality control and monitoring of cysteamine and cystamine in cosmetics.

Development of New Processes for the Decommissioning Decontamination and for Treatment and Disposal of the Secondary Low- and Intermediate-Level Radioactive Waste

  • John, Jan;Bartl, Pavel;Cubova, Katerina;Nemec, Mojmir;Semelova, Miroslava;Sebesta, Ferdinand;Sobova, Tereza;Sul'akova, Jana;Vetesnik, Ales;Vopalka, Dusan
    • 방사성폐기물학회지
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    • 제19권1호
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    • pp.9-27
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    • 2021
  • As an example of research activities in decontamination for decommissioning, new data are presented on the options for corrosion layer dissolution during the decommissioning decontamination, or persulfate regeneration for decontamination solutions re-use. For the management of spent decontamination solutions, new method based on solvent extraction of radionuclides into ionic liquid followed by electrodeposition of the radionuclides has been developed. Fields of applications of composite inorganic-organic absorbers or solid extractants with polyacrylonitrile (PAN) binding matrix for the treatment of liquid radioactive waste are reviewed; a method for americium separation from the boric acid containing NPP evaporator concentrates based on the TODGA-PAN material is discussed in more detail. Performance of a model of radionuclide transport, developed and implemented within the GoldSim programming environment, for the safety studies of the LLW/ILW repository is demonstrated on the specific case of the Richard repository (Czech Republic). Continuation and even broadening of these activities are expected in connection with the approaching end of the lifespan of the first blocks of the Czech NPPs.

Studies on the Macrocycle mediated Transport in a Bulk Liquid Membrane System of Transition Metal Ions

  • Cho, Moon-Hwan;Seon-Woo, Kie-Hwa;Heo, Moon-Young;Lee, In-Chong;Yoon, Chang-Ju;Kim, Si-Joong
    • Bulletin of the Korean Chemical Society
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    • 제9권5호
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    • pp.292-295
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    • 1988
  • Macrocyclic ligands have been studies as cation carriers in a bulk liquid membrane system. $Cu^{2+}$ has been transported using nitrogen substituted macrocycles as carriers and several transition metal ions($M^{n+}\;=\;Mn^{2+},\;Co^{2+},\;Ni^{2+},\;Cd^{2+},\;Pb^{2+}\;and\;Ag^{+}$) have been transported using $DBN_3O_2,\;DBN_2O_2,\;Me_6N_414C4$ and DA18C6 as carriers in a bulk liquid membrane system. Competitive $Cu^{2+}-M2^+$ transport studies have also been carried out for the same system. In single cation transport experiments, the best macrocyclic ligand for transport is a ligand that gives a moderately stable rather than very stable complex in the extraction. However, when both cations are present in the source phase, the cation which forms the most stable complex with carrier is favored in transport over other cations. Generally, the nitrogen substiituted macrocycles transport $Cu^{2+}$ selectively over $Mn^+$. Ligand structure, equilibrium constant (or stability constant) for complex formation, source phase pH and carrier concentration are also important parameters in transport experiments.