• Title/Summary/Keyword: liquid-liquid extraction (LLE)

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A Simple and Efficient Method to Determine Montelukast in Rat Plasma Using Liquid-Liquid Extraction and Tandem Mass Spectrometry

  • Kim, Dong Yoon;Lee, Hyo Chun;Jang, Yong Jin;Kim, Jin Hee;Lee, Ha Ryeong;Kang, Myung Joo;Choi, Yong Seok
    • Mass Spectrometry Letters
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    • v.11 no.4
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    • pp.71-76
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    • 2020
  • While montelukast (ML), a cysteinyl-leukotriene type 1 receptor (CysLT1) antagonist is widely used to treat symptoms of rhinitis or asthma, its formulations are mainly limited to solid preparation due to its instability. Recently, there have been attempts to develop various ML dosage forms, and this situation increases the demand of sensitive and creditable methods to determine ML in various samples such as plasma. Thus, here, a simple and efficient method to determine ML in rat plasma using liquid-liquid extraction (LLE) and multiple reaction monitoring was presented. The mixture of DCM:EtOAc (25:75, v/v), the optimized extract solvent for LLE was found to be effective to extract ML without hydrophilic salts and proteins from the sample with limited volume. Also, the use of zafirlukast, instead of expensive ML-d6, as the internal standard makes the present method economical. The developed method was successfully validated in terms of selectivity, matrix effects (-14.8--6.9%), linearity (r230.998 within 0.5-500 ng/mL), sensitivity (the limit of detection and the lower limit of quantitation, ≤0.5 ng/mL), accuracy (88.4-100.6%), precision (3.0-13.3%), and recovery (80.8-86.3%) by following the FDA guidelines. Finally, the applicability of the validated method to pharmacokinetics (PK) studies was confirmed by the successful determination of PK parameters through it following oral administration of Singulair® granule in rats. Therefore, the present method can contribute to the development of new ML formulations through its performance to determine ML in rat plasma efficiently and sensitively.

An extraction method and residues of benzimidazole fungicides in soybean sprouts (콩나물중 benzimidazole계 농약의 추출방법과 잔류성)

  • Park, Jun-Jo;Yong, Kum-Chan;Jeung, Jin-A
    • The Korean Journal of Pesticide Science
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    • v.4 no.1
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    • pp.26-31
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    • 2000
  • An analytical method was approached to determine the residues of benzimidazole fungicides in soybean sprouts and was compared with traditional solvent-based method of extraction, solid phase extraction(SPE) and matrix solid phase dispersion(MSPD). The recoveries of carbendazim for liquid-liquid extraction (LLE), SPE and MSPD in soybean sprouts were $69.25{\sim}79.16$, $79.99{\sim}90.42$ and $92.40{\sim}98.48%$, respectively. The recoveries of thiabendazole for LLE, SPE and MSPD in soybean sprouts were $64.86{\sim}83.26$, $79.12{\sim}94.04$ and $65.44{\sim}73.92%$, respectively. The residues of carbendazim by elapsed time under our cultivated soybean sprouts program found $0.10{\sim}0.25$ mg/kg after 5 days and trace concentration of carbendazim was detected after 7 days. Of the 448 samples analyzed, less than 1.5% had residues of carbendazim ranged from 0.05 to 0.37 mg/kg.

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Optimization of analytical conditions for the determination of nitrosamines in chlorinated tap water by high performance liquid chromatography (액체크로마토그래피를 이용한 수돗물 중 nitrosamine 화합물 분석의 최적화)

  • Han, Ki-Chan;Kim, He-Kap
    • Analytical Science and Technology
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    • v.23 no.6
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    • pp.551-559
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    • 2010
  • This study was conducted to establish an analytical method for the determination of seven nitrosamines in chlorinated tap water by precolumn derivatization followed by high performance liquid chromatography coupled with fluorescence detection. The derivatization procedure was optimized for denitrosation and dansylation, and then two extraction methods, liquid-liquid extraction (LLE) with dichloromethane and solid phase extraction (SPE), were compared. The SPE method employing the optimized derivation procedure showed higher extraction recovery (54.4-88.7%) and reproducibility (1.9-19.4%) than the LLE method (51.4-87.7% and 4.2-33.3%, respectively). The method detection limits were between 0.5 and 4.4 ng/L. When chlorinated water samples were collected from two treatment plants and ten household taps, and analyzed for nitrosamines, Nnitrosodimethylamine (NDMA) was the major compound found between 26.1 and 112 ng/L.

LLE and SLM studies for Pd(II) separation using a thiodiglycolamide-based ligand

  • Kumbhaj, Shweta;Prabhu, Vandana;Patwardhan, Anand V.
    • Membrane and Water Treatment
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    • v.9 no.6
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    • pp.463-471
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    • 2018
  • The present paper deals with the liquid-liquid extraction and flat sheet supported liquid membrane studies of Pd(II) separation from nitric acid medium using a novel synthesized ligand, namely, N,N,N',N'-tetraethyl-2,2-thiodiethanthiodiglycolamide (TETEDGA). The effect of various diluents and stripping reagents on the extraction of Pd(II) was studied. The liquid-liquid extraction studies showed complete extraction of Pd(II) in ~ 5 min. The influence of nitric acid and TETEDGA concentration on the distribution of Pd(II) has been investigated. The increase in nitric acid concentration resulted in increase in extraction of Pd(II). Stoichiometry of the extracted species was found to be $Pd(NO_3)_2{\cdot}TETEDGA$ by slope analysis method. Extraction studies with SSCD solution showed negligible uptake of Pt, Cr, Ni, and Fe, thus showing very high selectivity and extractability of TETEDGA for Pd(II). The flat sheet supported liquid membrane studies showed quantitative transport of Pd(II), ~99%, from the feed ($3M\;HNO_3$) to the strippant (0.02 M thiourea diluted in $0.4M\;HNO_3$) using 0.01 M TETEDGA as a carrier diluted in n-dodecane. Extraction time was ~160 min. Parameters such as feed acidity, TETEDGA concentration in membrane phase, membrane porosity etc. were optimized to achieve maximum transport rate. Permeability coefficient value of $2.66{\times}10^{-3}cm/s$ was observed using TETEDGA (0.01 M) as carrier, at 3 M, $HNO_3$ feed acidity across $0.2{\mu}m$ PTFE as membrane. The membrane was found to be stable over five runs of the operation.

The High-throughput Solid-Phase Extraction in the Field of Synthetic Biology: Applications for the Food Industry and Food Managements

  • Hyeri SEONG;Min-Kyu KWAK
    • The Korean Journal of Food & Health Convergence
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    • v.10 no.3
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    • pp.19-22
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    • 2024
  • The field of synthetic biology has emerged in response to the ongoing progress in the life sciences. Advances have been made in medicine, farming, eating, making materials, and more. Synthetic biology is the exploration of using living organisms to create new organisms. By manipulating specific genes to express targeted proteins, proteins can be created that are both productive and cost-effective. Solid-phase extraction (SPE) and liquid-liquid extraction (LLE) are employed for protein separation during the production process involving microorganisms. This study centers on Scanning Probe Microscopy (SPM) to showcase its utility in the food industry and food management. SPE is predominantly utilized as a pretreatment method to eliminate impurities from samples. In comparison to LLE, this method presents benefits such as decreased time and labor requirements, streamlined solvent extraction, automation capabilities, and compatibility with various other analytical instruments. Anion exchange chromatography (AEC) utilizes a similar methodology. Pharmaceutical companies utilize these technologies to improve the purity of biopharmaceuticals, thereby guaranteeing their quality. Used in the food and beverage industry to test chemical properties of raw materials and finished products. This exemplifies the potential of these technologies to enhance industrial development and broaden the scope of applications in synthetic biology.

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.

Monitoring and Development of Pretreatment Method for Perfluorinated Compounds in Fish Samples (어류에서의 과불화합물 분석을 위한 전처리법 확립 및 모니터링)

  • Heo, Jin-Ju;Lee, Ji-Woo;Kim, Seung-Kyu;Oh, Jeong-Eun
    • Journal of Korean Society of Environmental Engineers
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    • v.35 no.7
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    • pp.485-494
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    • 2013
  • An efficient extraction method was developed for the analysis of 16 perfluorinated compounds (PFCs) in fish samples. We compared the recoveries from the Ion-Pairing Extraction (IPE), Liquid-Liquid Extraction (LLE), Solid-Phase Extraction (SPE), IPE + SPE method with varying the injection time of the internal standard. As a result, IPE method with the internal standard before extraction was evaluated as the most effective pretreatment method. The RPM (Revolution Per Munite) and pH in IPE-before method were additionally adjusted and the more efficient pretreatment method was established. The total 33 fish samples including liver and gut samples were collected from Korean markets and analyzed PFCs with developed pretreatment method of this study. Total 16 PFC levels in fish samples ranged from ND to 1.67 ng/g with 100% detection frequency. The average PFCs concentrations of muscle, liver and gut samples from fish were compared and showed the following trend: liver (17.8 ng/g) > gut (13.3 ng/g) > muscle (1.67 ng/g). The PFC levels in fish samples were similar or lower than other available previous results of foreign studies.

Liquid-liquid extraction process for gas separation from water in polymeric membrane: Mathematical modeling and simulation

  • Salimi, Nahid;Moradi, Sadegh;Fakhar, Afsaneh;Razavi, Seyed Mohammad Reza
    • Membrane and Water Treatment
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    • v.7 no.5
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    • pp.463-476
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    • 2016
  • In this study, application of polypropylene hollow fiber membrane contactors for $CO_2$ removal from water in liquid-liquid extraction (LLE) mode was simulated. For this purpose, a steady state 2D mathematical model was developed. In this model axial and radial diffusion was considered to $CO_2$ permeation through the hollow fibers. $CO_2$ laden water is fed at a constant flow rate into the lumen side, permeated through the pores of membrane and at the end of this process, $CO_2$ solution in the lumen side was extracted by means of aqueous diethanolamine (DEA) and chemical reaction. The simulation results were validated with the experimental data and it was found a good agreement between them, which confirmed the reliability of the proposed model. Both simulation and experimental results confirmed the reduction in the percentage of $CO_2$ removal by increment of feed flow rate.

Simultaneous Analysis of Pesticide Priority Pollutants in Water Samples (수질 시료 중의 Pesticide Priority Pollutants 동시분석에 관한 연구)

  • Kim Kye-Young;Kim Chong-Hyeak;Lee Sueg-Geun
    • Journal of the Korean Chemical Society
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    • v.37 no.6
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    • pp.590-598
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    • 1993
  • The simultaneous analysis of samples, 16 organic pesticides in water among 129 priority pollutants listed by EPA, was performed by GC-ECD (electron capture detector) and GC/MS-SIM (selected ion monitoring). Two extraction procedures, liquid-liquid extraction (LLE) and solid-phase extraction (SPE), were studied as an extraction and concentration method. Accuracy and precision of the methods were measured by the calculation of mean recovery and mean relative standard deviation. Finally, the detection limits, the experimental limitations, and prospects were discussed.

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The Extraction and Derivatization of Organotins in Water Sample by Gas Chromatograph/Mass Spectrometer (기체크로마토그래프/질량분석기에 의한 물시료 중 Organotin의 추출 및 유도체 반응에 관한 연구)

  • Hong, Jee-Eun;Lee, Kang-Jin;Pyo, Hee Soo;Park, Song-Ja;Lee, Won
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.636-645
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    • 2000
  • A method is described for the determination of organotins in water samples by GC/MS. Optimized derivatization methods for ethylation and hydrogenation of organotins were surveyed according to various reaction conditions such as time, pH and concentration of reagents. The organotins were extracted with n-hexane in presence of 0.1% tropolone and hydrogenated with sodium borohydride. Extraction recoveries of organotins with hydrogenation were in the range of 61-112%. After ethylation, organotins in water samples were extracted by liquid-liquid extraction (LLE) and solid-phase extraction (SPE). Using LLE, extraction recoveries were in the range of 74-113%. The recoveries ranged from 61-97% in the case of SPE with styrene-divinylbenzene copolymers. Method detection limits of hydrogenated and ethylated organotins ranged from 0.05 to 0.5 ng/ml and from 0.02 to 0.05 ng/ml, respectively.

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