• Title/Summary/Keyword: Liquid Liquid Extraction

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Determination of 105 pesticide residues by GC/MS/MS (GC/MS/MS를 이용한 105종의 잔류농약 분석에 관한 연구)

  • Kim, W.S.;Do, J.A.;Lee, H.J.;Lee, J.Y.;Yang, S.J.;Lee, S.H.
    • Analytical Science and Technology
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    • v.23 no.4
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    • pp.395-404
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    • 2010
  • A multi-residual method using gas chromatography coupled with mass spectrometry (GC/MS/ MS) was developed for the analysis of 105 pesticides. This method was tested on lemons, beans and other vegetables. The pretreatment of these pesticides was performed by liquid-liquid partition followed by cleanup with solid phase extraction cartridge (SPE Florisil), after acetonitrile extraction from matrices and sodium chloride (15 g) addition. The recovery ranged from 71.1% to 126.0% except for azinphosmethyl, famoxadone, fenamidone, flufenoxuron and triadimefon in lemons and from 72.5% to 124.5% in bean. In lemon, the limit of detection (LOD) and limit of quantification (LOQ) were 0.001~150 ng/ mL and 0.004~500 ng/mL, respectively.

Antioxidant Activity and Standardization of Extraction Solvents of SJ004 (SJ004의 추출용매별 항산화 활성 및 표준화 연구)

  • Lee, Dae-Yeon;Jo, Ju-Hwi;Kim, Wan-Su;Lee, Ho-Sung;Yi, Young-Woo;Park, Sang-In;An, Keon-Sang;Lee, In-Hee
    • Journal of Korean Medicine Rehabilitation
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    • v.30 no.2
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    • pp.67-75
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    • 2020
  • Objectives SJ004 is a natural herbal medicine that contains Acyranthes japonica Nakai and Eucommia ulmoides Oliver traditionally used for joint and spinal diseases. This study aimed to establish an efficient method of extracting SJ004 to standardize using the yield, high-performance liquid chromatography (HPLC), and antioxidant assay. Methods SJ004 was extracted with distilled water, 70% and 100% of ethyl alcohol (EtOH). The method validation of 20-hydroxyecdysone and pinoresinol diglucoside was determined by HPLC-photo diode array and the content of SJ004 was calculated. The antioxidant activity of each extract was compared and measured using total flavonoids, total phenolic compounds, 2,2-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid), and ferric reducing antioxidant power according to the standard protocol. Results The yield was highest in pure water extract and lowest in 100% EtOH. But, the content of marker compounds indicating 20-hydroxyecdysone and pinoresinol diglucoside was highest in 100% EtOH extract. In the physiological activity measurement using antioxidant activity, 100% ethanol extract was highest. The limit of detection indicating 20-hydroxyecdysone and pinoresinol diglucoside were analyzed 0.33 ㎍/mL, 0.1616 ㎍/mL, and the limit of quantification were analyzed 1.01 ㎍/mL and 0.49 ㎍/mL respectively. Conclusions The experimental results showed that the extraction conditions have a significant effect on content of marker compounds and antioxidant activity. As a result of method validation, SJ004 was standardized by 20-hydroxyecdysone and pinoresinol diglucoside.

Comparison of Volatile Flavor Compounds in Commercial Crab-like Flavorants by Analyzing Methods (분석방법에 따른 시판 게향료의 휘발성 향기성분 비교)

  • Cha, Yong-Jun;Cho, Woo-Jin;Jeong, Eun-Jeong
    • Journal of Life Science
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    • v.16 no.7 s.80
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    • pp.1243-1249
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    • 2006
  • Volatile flavor compounds in commercial crab-like flavorants were compared by mean of solid phase microextraction(SPME) and liquid continuous extraction (LLCE)/GC/MSD methods. A total of 86 volatile flavor compounds were detected. Of these, 71 were positively identified consisting mainly of sulfur-containing compounds (13), aldehydes (3), ketones (2), esters (26), alcohols (5), aromatic compounds (3), terpenes (8), acids (2) and miscellaneous compounds (9). SPME method was more effective than LLCE method in detection of volatile components in commercial crab-like flavorants. Eight S-, N-containing compounds such as dimethyl sulfide, dimethyl disulfide, dipropyl disulfide, 3-(methylthio)propyl acetate, 3-(methylthio) propanal, 3-(methylthio) propanol, 2-methyl-3-(methylthio) pyrazine and 2-methyl-5-(methylthio) pyrazine, 8 esters such as styrallyl acetate, ethyl acetate, isoamyl acetate, benzyl acetate, ethyl pentanoate, butyl pentanoate, isoamyl pentanoate and furfuryl acetate were considered as major components in crab-like flavorants.

Nucleotide Analysis in Korean Dairy Products Using High- Performance Liquid Chromatography with Diode Array Detector

  • Won, Jong-Eun;Bang, Han-Yeol;Kwak, Byung-Man;Park, Jong-Su;Kim, Gui-Ran;Kwon, Joong-Ho
    • Food Science of Animal Resources
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    • v.39 no.1
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    • pp.93-101
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    • 2019
  • Nucleotides play important roles in numerous intracellular biochemical processes and are used in infant formulas and other dairy products. However, domestic analytical methods for assessing nucleotide content in products have not yet been established, and therefore, methods for determining nucleotide content are urgently required. A rapid and simple analytical method for determining the content of five types of nucleotides in dairy products was improved using solid phase extraction clean-up and high-performance liquid chromatography with diode array detector. The extraction solvent used in the AOAC method was not well dissolved and was changed to hydrophilic EDTA-Na. In addition, the results obtained using the isocratic elution method and a single wavelength were similar to those obtained using the AOAC method, and the time taken for analysis was shortened from 40 min to 25 min. The process of method validation revealed the following parameters: accuracy (84.69%-102.72%), precision (1.51%-6.82%), linearity (0.999), and limit of detection (cytidine 5'-monophosphate, 0.09 mg/L; uridine 5'-monophosphate, 0.11 mg/L; adenosine 5'-monophosphate, 0.12 mg/L; guanosine 5'-monophosphate, 0.11 mg/L; and inosine 5'-monophosphate, 0.14 mg/L). The method was also used to determine the nucleotide concentration in 25 samples (infant formulas, 1.99-29.39 mg/100 g; and cow milk, 0.28-0.83 mg/100 g). The newly improved method was appropriate for analyzing nucleotides in infant formulas and other dairy products faster when compared to conventional methods.

Simultaneous Quantitative Determination of Nine Hallucinogenic NBOMe Derivatives in Human Plasma Using Liquid Chromatography Tandem Mass Spectrometry

  • Seo, Hyewon;Yoo, Hye Hyun;Kim, Young-Hoon;Hong, Jin;Sheen, Yhun Yhong
    • Mass Spectrometry Letters
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    • v.10 no.1
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    • pp.18-26
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    • 2019
  • We developed a bioanalytical method for simultaneous determination of nine NBOMe derivatives (25H-NBOMe, 25B-NBOMe, 25E-NBOMe, 25N-NBOMe, 25C-NBOH, 25I-NBOH, 25B-NBF, 25C-NBF, and 25I-NBF) in human plasma using liquid chromatography tandem mass spectrometry (LC-MS/MS). Human plasma samples were pre-treated using solid-phase extraction. Separation was achieved on a C18 column under gradient elution using a mobile phase containing 0.1% formic acid in acetonitrile and 0.1% formic acid in water at a flow rate of 0.3 mL/min. Mass detection was performed in the positive ion mode using multiple reaction monitoring. The calibration range was 1-100 ng/mL for all quantitative analytes, with a correlation coefficient greater than 0.99. The intra- and inter-day precision and accuracy varied from 0.85 to 6.92% and from 90.19 to 108.69%, respectively. The recovery ranged from 86.36 to 118.52%, and the matrix effects ranged from 27.09 to 99.72%. The stability was acceptable in various conditions. The LC-MS/MS method was validated for linearity, accuracy, precision, matrix effects, recovery and stability in accordance with the FDA guidance. The proposed method is suitable for reliable and robust routine screening and analysis of nine NBOMe derivatives in forensic field.

Separation of Uranium(VI) and Vanadium(V) from Sulfuric Acid Media by Amine Based Extractants through Liquid-liquid Extraction Technique (황산 용액으로부터 아민계 추출제의 액-액 추출법에 의한 우라늄(VI)과 바나듐(V)의 분리)

  • Jeon, Jong-Hyuk;Lee, Jin-Young;Kim, Joon Soo;Yoon, Ho-Sung;Jyothi, Rajesh Kumar
    • Resources Recycling
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    • v.30 no.4
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    • pp.64-74
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    • 2021
  • The importance of uranium metal is growing day by day in light of its increasing global demand for fulfilling societal needs through atomic power programs. Considering the high demand for uranium, it is necessary to find innovative hydrometallurgical techniques to separate uranium from other associated elements, especially vanadium. This study deals with the separation of uranium(VI) and vanadium(V) from sulfuric acid solutions using commercial amine-based extractants diluted in kerosene. The concentrations of the sulfuric acid solutions ranged from 0.005 to 5.0 mol/L. The effect of extractant concentration ranging from 0.005 to 0.2 mol/L was studied. The temperature was maintained at 25℃ and the experiment was performed for 30 min at an aqueous: organic phase ratio of 1 (A:O = 1:1). The calculated separation factors (SFs) are presented and comparisons are made among all the experiments.

Improved HPLC-UV method for determination of five synthetic dyes in Typha orientalis

  • Ko, Kyung Yuk;Choi, Eun Young;Jeong, Se Hee;Paek, Ock jin;Lee, Chan;Heo, Huijin;Oh, She-Wook;Lee, Chulhyun;Kang, Juhye;Cho, Sooyeul
    • Analytical Science and Technology
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    • v.34 no.4
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    • pp.160-171
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    • 2021
  • Synthetic azo dyes are used extensively in herbal medicines to render the medicines more visually attractive to consumers. This study developed and validated a rapid high-performance liquid chromatography (HPLC) method to determine whether synthetic colorants such as Tartrazine, Auramine O, Metanil yellow, Sunset yellow, and Orange II are used extensively in Typha orientalis. To increase the recovery of the synthetic dyes, this method employed containing 50 mM ammonium acetate in 70 % methanol at first extraction and 100 mM HCl in 70 % methanol at second extraction. Five synthetic pigments in Typha orientalis were separated by gradient elution with a mobile phase consisting of acetonitrile and 50 mM ammonium acetate in distilled water at ultra-violet (UV) detection 428 nm or 500 nm. Additionally, this study established the liquid chromatography tandem mass spectrometry (LC-MS/MS) method to confirm positive samples suspected by HPLC results. The HPLC-UV method had good linearity, indicating r2> 0.999. The recoveries of the samples spiked with three different concentration ranged from 73.8~91.5 %, and relative standard deviation values indicated 0.2~5.2 %. The established LC-MS/MS could successfully identify the synthetic pigments in herbal medicine samples. The study demonstrates that Typha orientalis adulterated by yellowish synthetic dyes can be successfully distinguished when using the HPLC-UV method.

Study on Reaction Behavior of Mg-FeB Phase for Rare Earth Elements Recovery from End-of-life Magnet

  • Sangmin Park;Dae-Kyeom Kim;Rongyu Liu;Jaeyun Jeong;Taek-Soo Kim;Myungsuk Song
    • Journal of Powder Materials
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    • v.30 no.2
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    • pp.101-106
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    • 2023
  • Liquid metal extraction (LME), a pyrometallurgical recycling method, is popular owing to its negligible environmental impact. LME mainly targets rare-earth permanent magnets having several rare-earth elements. Mg is used as a solvent metal for LME because of its selective and eminent reactivity with rare-earth elements in magnets. Several studies concerning the formation of Dy-Fe intermetallic compounds and their effects on LME using Mg exist. However, methods for reducing these compounds are unavailable. Fe reacts more strongly with B than with Dy; B addition can be a reducing method for Dy-Fe intermetallic compounds owing to the formation of Fe2B, which takes Fe from Dy-Fe intermetallic compounds. The FeB alloy is an adequate additive for the decomposition of Fe2B. To accomplish the former process, Mg must convey B to a permanent magnet during the decomposition of the FeB alloy. Here, the effect of Mg on the transfer of B from FeB to permanent magnet is observed through microstructural and phase analyses. Through microstructural and phase analysis, it is confirmed that FeB is converted to Fe2B upon B transfer, owing to Mg. Finally, the transfer effect of Mg is confirmed, and the possibility of reducing Dy-Fe intermetallic compounds during LME is suggested.

Evaluation of Efficiency of SVE from Lab-scale Model Tests and Numerical Analysis (실내모형시험과 수치해석을 통한 SVE의 효율성 평가)

  • Suk, Heejun;Seo, Min Woo;Ko, Kyung-Seok
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.28 no.1B
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    • pp.137-147
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    • 2008
  • Soil Vapor Extraction (SVE) has been extensively used to remove volatile organic compounds (VOCs) from the vadoze zone. In order to investigate the removal mechanism during SVE operation, laboratory modeling experiments were carried out and tailing effect could be observed in later stage of the experiment. Tailing effect means that removal rate of contaminants gets significantly to decrease in later stage of SVE operation. Also, mathematical model simulating the tailing effect was used, which considers rate-limited diffusion in a water film during mass transfer among gas, liquid, and solid phases. Measurement data obtained through the experiment was used as input data of the numerical analyses. Sensitivity analysis was performed to examine the effect of each parameter on required time to reach final target concentration. Finally, it was found that the concentration in the soil phase decreased significantly with a liquid and gas diffusion coefficient larger, actual path length shorter, and water saturation smaller.

Development of an Automatic PCR System Combined with Magnetic Bead-based Viral RNA Concentration and Extraction

  • MinJi Choi;Won Chang Cho;Seung Wook Chung;Daehong Kim;Il-Hoon Cho
    • Biomedical Science Letters
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    • v.29 no.4
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    • pp.363-370
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    • 2023
  • Human respiratory viral infections such as COVID-19 are highly contagious, so continuous management of airborne viruses is essential. In particular, indoor air monitoring is necessary because the risk of infection increases in poorly ventilated indoors. However, the current method of detecting airborne viruses requires a lot of time from sample collection to confirmation of results. In this study, we proposed a system that can monitor airborne viruses in real time to solve the deficiency of the present method. Air samples were collected in liquid form through a bio sampler, in which case the virus is present in low concentrations. To detect viruses from low-concentration samples, viral RNA was concentrated and extracted using silica-magnetic beads. RNA binds to silica under certain conditions, and by repeating this binding reaction, bulk samples collected from the air can be concentrated. After concentration and extraction, viral RNA is specifically detected through real-time qPCR (quantitative polymerase chain reaction). In addition, based on liquid handling technology, we have developed an automatic machine that automatically performs the entire testing process and can be easily used even by non-experts. To evaluate the system, we performed air sample collection and automated testing using bacteriophage MS2 as a model virus. As a result, the air-collected samples concentrated by 45 times then initial volume, and the detection sensitivity of PCR also confirmed a corresponding improvement.