• Title/Summary/Keyword: Liquid Liquid Extraction

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Levels of Perfluorinated Compounds in Liquid Milk Products in Korea

  • Park, Na-youn;Kho, Younglim;Kim, Junghoan
    • Journal of Food Hygiene and Safety
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    • v.36 no.4
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    • pp.310-315
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    • 2021
  • This study was carried out to monitor the level of 17 perfluorinated compounds (PFCs) present in liquid milk products sold on the Korean market. The liquid milk samples were extracted via liquid-liquid extraction and analyzed by LC-MS/MS. Excellent linearity over the calibration range (r2>0.99), and the limit of quantification of perfluorooctane sulfonate (PFOS) was 0.021 ng/g, and perfluorotetradecanoic acid (PFOA) was 0.057 ng/g. The accuracy was in the range of 72.5-115.3%, and the precision was under 20%. The preprocessing method for this experiment is considered appropriate for analysis of milk samples. The proposed analytical method was applied for the determination of PFCs in 98 liquid milk product samples, and the average content of total PFCs was 0.6576 ng/mL. PFOA and PFOS were detected in most samples, and their levels were less than 0.1 ng/mL, which was lower than those in other studies.

Effects of Main Constituents of W/O Emulsion on Removal of Acetic Acid in a Simulated Hemicellulosic Hydrolysate (W/O 에멀젼의 주요 구성 성분들이 모사 헤미셀룰로오스 가수분해액에 있는 초산의 제거에 미치는 영향)

  • Lim, Sung Jin;Lee, Sang Cheol
    • Korean Chemical Engineering Research
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    • v.52 no.6
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    • pp.789-795
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    • 2014
  • Acetic acid is the most abundant and serious ethanol fermentation inhibitor in dilute-acid hemicellulosic hydrolysates. A mixture of xylose, acetic acid and sulfuric acid was chosen as a simulated hemicellulosic hydrolysate so as to find an optimal separation system to selectively remove acetic acid from the hydrolysates. In order to attain the purpose, emulsion liquid membrane was applied to removal of acetic acid from the simulated hemicellulosic hydrolysate. The effects of main constituents of water-in-oil (W/O) emulsion, such as amine extractant type, surfactant composition, additive type, and type and concentration of stripping agent, on extraction of acetic acid, xylose, and sulfuric acid in the simulated hemicellulosic hydrolysate were investigated. Under specific experimental conditions, degree of extraction of acetic acid was higher than 95% while loss of xylose was insignificant, which means that the current emulsion liquid membrane can be an economically feasible process.

A Study of Analytical Method for Trace Metal Ions in Whole Blood and Urine by Inductively Coupled Plasma-Mass Spectrometry using Solid-Liquid Extraction Technique (유도결합 플라스마-질량분석법과 고체-액체 추출법을 이용한 혈액 및 소변중 미량금속의 분석에 관한 연구)

  • Lee, Won;Hur, Young-Hoe;Park, Kyung-Su
    • Analytical Science and Technology
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    • v.11 no.4
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    • pp.281-291
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    • 1998
  • An analytical method for the simultaneous measurement of trace Cu, Sn, and Bi in blood and urine has been investigated by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). Microwave oven was used for the pretreatment of blood samples using nitric acid and hydrogen peroxide in a closedvessel digestion system with 1 mL whole blood for 8 minutes. Amberlite IRC-718 resin was used as a solid phase in solid-liquid extraction technique for the removal of matrix interferences such as Na, S, P, and other polyatomic ion species. Detection limits for Cu, Sn, and Bi by this method were 0.000375 ng/mL, 0.000297 ng/mL, and 0.000174 ng/mL, respectively. Recoveries of 99.1% for Cu, 102.5% for Sn, and 98.4% for Bi were obtained for the standard spiked NIST SRM 955a blood sample. The developed method was applied for whole real blood and urine samples.

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Simultaneous analysis of sulfonamides in beef and pork by high performance liquid chromatography and electrospray ionization mass spectrometry (HPLC와 LC/MS에 의한 식육내 잔류 설파제의 동시 분석법)

  • 정봉수;박준조;금모래;김인경;박병옥;한정희
    • Korean Journal of Veterinary Service
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    • v.27 no.1
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    • pp.17-29
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    • 2004
  • A multiresidual analysis was performed to determine 12 sulfonamides(sulfacetamide, sulfadiazine, sulfisomidine, sulfathiazole, sulfapyridine, sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfisoxazole, sulfamethoxazole, sulfaquinoxaline, and sulfadimethoxine) in beef and pork simultaneously. The multiresidual analysis for the sulfonamides currently used was able to analyze 5 kinds of sulfonamides at the same time. The method of this 12 sulfonamides multiresidual analysis in this study was matrix solid-phase dispersion(MSPD) by high performance liquid chromatography (HPLC) and liquid chromatography mass spectrometry (LC/MS). The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM: Ethylacetate(3:1), DCM:EA(9:1). Also, samples (84 beef and 205 pork samples) which were positive by EEC-4 plate test from 2001 to 2003 were tested to investigate the kinds of sulfonamides using HPLC. The results from the study were as follows; 1. The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM:Ethylacetate(3:1), DCM:EA(9:1). The method of extraction solvent with DCM:ethyl acetate(9:1) was the most excellent(87.7∼99.3%) in separation and reappearance. 2. In the LC/MS analysis. of sulfonamides, signal to noise ratio was showed relatively high in the positive mode and special ion in the quality analysis was determined via [M+H]$\^$+/ and m/z 156. A spectrum of sulfonamides was showed from all 12 sulfonamides. 3. The samples positive by the EEC-4 plate, a screening test method, were categorized by sulfonamides through Charm II and confirmed the kinds of sulfonamides through HPLC. 1) Among 84 beef samples positive by EEC-4 plate, 20 samples were positive by Charm II and identified as 7 sulfamethazine, 9 sulfadimethoxine, 1 sulfamonomethoxine and 3 unknown status. 2) Among 205 pork samples positive by EEC-4 plate, 42 samples were positive by Charm II and identified as 19 sulfamethazine, 1 sulfadimethoxine, 4 sulfamonomethoxine and 5 unknown status.

Development of a Sensitive Analytical Method of Polynemoraline C Using LC-MS/MS and Its Application to a Pharmacokinetic Study in Mice

  • Pang, Minyeong;Lee, Jaehyeok;Jeon, Ji-Hyeon;Song, Im-Sook;Han, Young Taek;Choi, Min-Koo
    • Mass Spectrometry Letters
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    • v.12 no.4
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    • pp.200-205
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    • 2021
  • Polynemoraline C, a pyridocoumarin alkaloid, exhibits anticholinergic, anti-inflammatory, antitumor, and antimicrobial activities. A sensitive analytical method of polynemoraline C in mouse plasma was developed and validated using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Polynemoraline C and 13C-caffeine (internal standard) in mouse plasma were extracted using a liquid-liquid extraction method coupled with ethyl acetate. This extraction method resulted in high and reproducible extraction recovery in the range of 73.49%-77.31% with no interfering peaks around the peak retention time of polynemoraline C and 13C-caffeine. The standard calibration curves for polynemoraline C were linear over the range of 0.5-200 ng/mL with r2 > 0.985. The accuracy, precision, and the stability of the data were within acceptable limits on the FDA guideline. After intravenous and oral administration of polynemoraline C at doses of 5 and 30 mg/kg, respectively, the present method was successfully applied to the pharmacokinetic study of polynemoraline C. Polynemoraline C in mouse plasma showed a multi-exponential elimination pattern with a high volume of distribution values. This compound's absolute oral bioavailability was found to be 17.0%. Polynemoraline C's newly developed LC-MS/MS method can be used for further studies on the efficacy, toxicity, and biopharmaceutics of polynemoraline C, as well as its pharmacokinetic studies.

The study on the pretreatments for the analys is of benzidine metabolites in urine (요중 벤지딘 대사물질 분석의 전처리 및 저장방법에 따른 회수율 비교)

  • Kim, Hyun Soo;Won, Jonguk;Kim, Chi Nyon;Roh, Jaehoon
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.9 no.2
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    • pp.100-109
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    • 1999
  • This study evaluates the pretreatment for analysis of benzidine metabolites in urine by measuring the recovery rates according to the temperature and periods of storage of the urine. By the solid phas e extraction, the recovery rates of basic hydrolysis are benzidine 67.4 %, monoacetylbenzidine 105.1 %, and diacetylbenzidine 115.8 %, respectively. By the liquid extraction, the recovery rates of back-extraction into 0.1 M perchloric acid are benzidine 105.7%, monoacetylbenzidine 94.2 %, diacetylbenzidine 72.8 %, respectively. The difference of the recovery rates between the back-extraction into 0.1 M HCl and 0.1 M perchloic acid after basic hydrolysis are 101 % and 98.8 %, respectively. When the recovery rates of the urinary s amples of pH 3, pH 7, pH 12 at $25^{\circ}C$ and $-76^{\circ}C$ are compared for four weeks, there are no differences according to the temperature and the periods of storage. The above results show that the solid phase extraction and back-extraction by 0.1 M perchloric acid after basic hydrolys is are suitable for the analysis of benzidine metabolites. There are no difference of the recovery rates of the urinary samples stored at $25^{\circ}C$ and $-76^{\circ}C$ at pH 3, pH 7, pH 12, respectively for 28 days.

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Developement of Quantitative Extraction Method of Amygdalin without Enzymatic Hydrolysis from Kyonin(Armeniacae Semen) by High Performance liquid Chromatography

  • Kim, Dong-Min;Hong, Seon-Pyo
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.388.3-389
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    • 2002
  • Kyonin(Armeniacae Semen)is the herb medicine that contains amygdalin as a major ingredient. Amygdalin in water is decomposed into benzaldehyde. HCN. and glucose by emulsin. a hydrolysis enzyme in kyonin. A useful and practical method for the optimum extraction condition of amygdalin without enzymatic hydrolysis is required. The extraction yield of amygdalin of natural formula kyonin was 0.5% from crude powers. 0.7% from small pieces. 1.2% from half pieces and 2.7% from whole pieces. (omitted)

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Studies on Preparation of Boron Compounds from Colemanite Ore : Preparation of Boric Acid and Reaction Mechanism (I) (Colemanite 광물로부터 붕소화합물의 제조에 관한 연구 : 붕산제조 및 반응기구 (I))

  • Choi, Byung-Hyun;Lim, Hyung-Mi;Jee, Mi-Jung;Jang, Jae-Hun;Paik, Song-Hoo;Lee, Mi-Jai
    • Journal of the Korean Ceramic Society
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    • v.41 no.10 s.269
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    • pp.756-765
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    • 2004
  • We present extraction process and reaction mechanism of boric acid from one of calcium borate ores, colemanite by reaction with sulfuric acid. Colemanite has been fully decomposed under pH 5 with sufficiency amount of sulfuric acid, more than the amount stoichiometrically required. Calcium sulfate was separated out, leaving boron in the liquid phase after sulfuric acid addition. The extraction process of boric acid was affected by dissolution temperature and time, amount of sulfuric acid and ammonium sulfate, pH and a degree of concentration before recrystallization. The $SiO_2$ of the impurities which colemanite contains was insoluble so that it was separated out with calcium sulfate from liquid phase. The species of $CaO,\;Al_2O_3,\;Fe_2O_3,\;MgO$ were remained in a liquid phase after reaction with sulfuric acid. These impurities were separated out by addition of ammonia to the liquid phase, funhermore, boric acid was produced by process of pH adjustments and acidification, concentration, and recrystallization.

Comparative Evaluation of the Analytical Methods used to Determine Pesticide Residues in Milk via Dispersive Solid Phase Extraction (Dispersive Solid Phase Extraction을 사용한 우유 내 잔류농약 다성분 동시 분석법 비교연구)

  • Oh, Nam Su;Shin, Yong Kook;Lee, Ji Young;Baick, Seung Chun
    • Journal of Dairy Science and Biotechnology
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    • v.33 no.1
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    • pp.27-34
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    • 2015
  • The aim of this study was to optimize a simple, fast, and economic analytical method for the simultaneous determination of various pesticides (aldrin, p,p'-DDT, o,p'-DDT, p,p'-DDE, ${\alpha}$-endosulfan, ${\beta}$-endosulfan, dieldrin, heptachlor, permethrin, chlordane, deltamethrin, diazinon, bifenthrin, methoprene, propargite, fenpropathrin, cypermethrin, fenvalerate, and fenpropathrin) in milk by using dispersive solid phase extraction (SPE). In this study, two different extraction methods (low temperature cleanup and liquid-liquid partitioning), which were followed by a cleanup process based on dispersive-SPE, were evaluated and compared for the 19 pesticides. The results for all the pesticides were determined by gas chromatography mass spectrometry (GC/MS) with selected-ion monitoring mode, and the matrix effect of the method was evaluated. Comparison of these approaches yielded higher and more consistent recoveries of most pesticides at fortification levels of $1{\mu}g/mL$ using low-temperature fat precipitation, followed by cleanup process based on dispersive-SPE with PSA and C18 as sorbents, than other preparation process. The relative standard deviation was <20 % and the combination of this method were very effective for the cleanup.

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Recovery of the Vanadium and Tungsten from Spent SCR Catalyst Leach Solutions by Hydrometallurgical Methods (SCR 폐촉매 침출액으로부터 습식제련법에 의한 바나듐, 텅스텐의 회수)

  • Choi, In-Hyeok;Moon, Gyeonghye;Jeon, Jong-Hyuk;Lee, Jin-Young;Jyothi, Rajesh Kumar
    • Resources Recycling
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    • v.29 no.2
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    • pp.62-68
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    • 2020
  • In new millennium, wide-reaching demands for selective catalytic reduction (SCR) catalyst have been increased gradually in new millennium. SCR catalyst can prevent the NOx emission to protect the environment. In SCR catalyst the main composition of the catalyst is typically TiO2 (70~80%), WO3 (7~10%), V2O5 (~1%) and others. When the SCR catalysts are used up and disposed to landfills, it is problematic that those should exist in the landfill site permanently due to their extremely low degradability. A new advanced technology needs to be developed primarily to protect environment and then recover the valuable metals. Hydrometallurgical techniques such as leaching and liquid-liquid extraction was designed and developed for the spent SCR catalyst processing. In a first stage, V and W selectively leached from spent SCR catalyst, then both the metals were processed by liquid-liquid extraction process. Various commercial extractants such as D2EHPA, PC 88A, TBP, Cyanex 272, Aliquat 336 were tested for selective extraction of title metals. Scrubbing and stripping studies were tested and optimized for vanadium and tungsten extraction and possible separation. 3rd phase studies were optimized by using iso-decanol reagent.