• Proceedings of the Korean Radioactive Waste Society Conference
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• 2004.02a
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• pp.245-256
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• 2004

The extraction of three kinds of amido podands, N,N,N'N'-tetrabutyl-3-oxa-pentanedi- amide (TBDGA), N,N,N'N'-tetra-isobutyl-3-oxa-pentanediamide(TiBDGA) and N,N,N'N'-tetra- butyl-3,6-dioxa-oct-anediam- ide(TBDOODA) on U(VI),Pu(IV), Am(III), Eu(III) and other metal ions is studied in nitric acid solutions. 40%octanol-kerosene is chosen as diluents to eliminate third phase and emulsion. TBDGA and TiBDGA show extraction selectivity to An(III) and Ln(III) much higher than to U(VI) and Pu(IV). Fe, Ru and Mo is poorly extracted by the three kinds of amid podands in 2~3mol/L $HNO_3$ solutions. Aiming to eliminate interface crude when using simulated HLLW solution in the system of 0.2mol/L TBDGA/Octanol＋kerosene, acetohydroxyamic acid was adapted. Distribution ratio of zirconium was decreased when adding acetohydroxyamic acid in aqueous solution, and interface crude disappeared as mixing extractant with HLLW. The counter-current extraction test is carried out in a set of miniature mixer-settler, with 0.2mol/L TBDGA/ 40% octanol-kerosene as extractant to separate U(VI), Pu(IV), Am(III) and Eu(III) from simulated high level liquid waste(HLLW) solution. In battery A, lanthanides and actinides are coextracted into organic phase with the recovery of 99.98% for U(Ⅵ), >99.99% for Pu(IV), and >99.99% for Am(III) and Eu(III) respectively. In battery R1, 99.99% U, 86.2% Pu and a part of Am or Eu are stripped into aqueous phase by 0.2mol/L acetohydroxyamic acid (AHA) in 0.01mol/L $HNO_3$ solution. In battery $R_2$, Am, Eu and remained Pu are completely back-extracted by 0.2mol/L AHA. This separation process contains no salt reagent, and it is not necessary to dilute HLLW feed.

• Environmental Engineering Research
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• v.14 no.4
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• pp.250-254
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• 2009

Contamination of microcystins, a family of heptapeptide hepatotoxins, in eutrophic water bodies is a worldwide problem. Due to their poisoning effects on animals and humans, there is a requirement to characterize and quantify all microcystins present in a sample. As microcystins are, for most part, intracellular toxins produced by some genera of cyanobacteria, lysing cyanobacterial cells to release all microcystins is considered an important step. To date, although many cell lysis methods have been used, little work has been conducted comparing the results of those different methods. In this study, various methods for cell lysis and toxin extraction from the cell lysates were investigated, including sonication, bead beating, freeze/thaw, lyophilization and lysing with TritonX-100 surfactant. It was found that lyophilization, followed by extraction with 75% methanol, was the most effective for extracting toxins from Microcystis aeruginosa cells. Another important step prior to the analysis is removing impurities and concentrating the target analyte. For these purposes, a C18 Sep-Pak solid phase extraction cartridge was used, with the percentage of the eluent methanol also evaluated. As a result, methanol percentages higher than 75% appeared to be the best eluting solvent in terms of microcystin-leucine-arginine (MC-LR) recovery efficiency for the further chromatographic and mass spectrometric analyses.

• Journal of Korean Society on Water Environment
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• v.32 no.6
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• pp.600-627
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• 2016

Korea is one of the countries with a large veterinary antibiotics market, although antimicrobial resistance in bacteria is becoming a serious issue in many countries. The Korean government started to take interest in estimating the effects of livestock manure on rivers and agricultural soils and in monitoring of heavy metals, organic pollutants and antibiotics in the ambient water and soil. In this paper, pre-treatment methods to separate the selected antibiotics from solid samples were reviewed. It is essential to select an efficient and appropriate procedure for pre-treatment due to the high proportion of proteins and organics in biosolid samples. Pre-treatment consists of extraction followed by clean-up. Initially, homogenized samples were extracted by sonication, mechanical agitation or pressurized liquid extraction with methanol/acetonitrile/water mixture under acidic/basic conditions depending on the compound. However, aminoglycosides and colistin were extracted with 5% trichloroacetic acid and HCl, respectively. Since the ${\beta}-lactams$ are easily decomposed in acidic and basic conditions, they were extracted in neutral pH. Filtration with a membrane (pore size, $0.2{\mu}m$) or solid phase extraction with HLB and methanol, as eluents, was normally applied for the clean-up. At least, three different pre-treatment procedures should be adopted to screen all the selected antibiotics in solid samples.

• Korean Journal of Medicinal Crop Science
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• v.22 no.2
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• pp.147-153
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• 2014

The Ponciri fructus immaturus (Poncirus trifoliata Rafinesque) has been used in oriental medicine for uterine contraction, stomachache, abdominal distension and cardiovascular diseases. Two main compounds, poncirin and naringin were successfully analyzed by high performance liquid chromatography (HPLC) and carried out method validation according to ICH guideline. A successful resolution and retention times were obtained with a $C_{18}$ reversed phase column, at an $1m{\ell}min^{-1}$ flow rate, with a gradient elution of a mixture of methanol, water and acetonitrile. Poncirin and naringin showed good linearity ($R^2$ > 0.999) in relatively wide concentration ranged. The recovery of each compound was 95.81 ~ 101.48% with R.S.D. values less than 1.0%. The application of ultrasound-assisted extraction was shown to be more efficient in extracting poncirin and naringin from Ponciri fructus immaturus. The predicted optimal poncirin and naringin yield were poncirin 2.15%, naringin 1.65% under an extraction temperature of $40^{\circ}C$, an extraction time of 10 min in a solvent of 70% methanol.

• Journal of the Korean Chemical Society
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• v.34 no.6
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• pp.663-672
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• 1990

The extraction of ginseng saponins with near critical or supercritical ammonia(SCF-NH$_3$) was carried out at 80$^{\circ}C$-160$^{\circ}C$ and ammonia densities of 339.8-525 $mg/cm^3$. In order to evaluate brownish color of white ginseng extracts, a spetrophotometric method was applied in ultraviolet and visible range. The extractibilities of ginseonoside $Rb_1$, -$Rb_2$, -Rc, -Rd, -Re, -Rf, $-Rg_1$, and $-Rg_2$ were determined by high performance liquid choromatography. The best extractability was 7.36% at 133$^{\circ}C$ and 403 $\pm$ 24.605 $mg/cm^3$. In the case of the high extraction temperature, it is thought that extraction times can be reduced and the selectivity of protopanaxatriol can be increased. The brownish color of extracts is affected by temperature and extractability. When extraction temperature is between 132$^{\circ}C$ and 140$^{\circ}C$, it is shown that the range is the retrograde region where extractablility decrease with increasing temperature.

• Korean Journal of Food Science and Technology
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• v.46 no.4
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• pp.465-469
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• 2014

The extraction of flavanones such as naringin, narirutin, naringenin, hesperidin, and hesperetin from grapefruit peels was performed using subcritical water extraction (SWE), hot water extraction, and conventional methods such as methanol and ethanol extraction. We analyzed the total flavanone content using high-performance liquid chromatography (HPLC) for each extracting method. Among the three methods, SWE was the optimal method with optimal operating conditions of $170^{\circ}C$ temperature and 10 min operating time. The maximum total flavanone extracted was $86.539{\pm}3.52mg/g$ grapefruit peels. Moreover, we treated the extracts with 60% ${\beta}$-cyclodextrin and then analyzed the surface structure of the encapsulated compounds by field emission-scanning electron microscopy (FE-SEM). The results indicated that the encapsulation in ${\beta}$-cyclodextrin improved solubilization, and the inclusion complex could serve as food supplements.

• Applied Chemistry for Engineering
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• v.30 no.1
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• pp.34-38
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• 2019

A cement industrial by-product was used as a Ca source for the carbonation process. It was confirmed that the most of cement industrial by-products was composed of CaO and KCl through ICP and XRD analyses. The optimal extractant type and concentration was 1.5 M of hydrochloric acid, and the solid/liquid ratio was 0.1 g/mL. It was assumed that the cation extraction efficiency was dependent of the pair ions and their binding formation and also the solubility from extraction efficiency results by varing extractants. After extraction process, it was also confirmed that the cation could be selectively separated from the solution with respect to the kind of additives and the injection order. When NaOH was injected into the solution to control pH values ranging from 9.5 and 13, impurities and $Ca(OH)_2$ were precipitated, whereas the separated K ion was precipitated in the form of KCl under the injected $C_2H_5OH$.

• Journal of the Korean Chemical Society
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• v.63 no.6
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• pp.415-419
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• 2019

Fipronil is an insecticide that belongs to the N-phenylpytazole and has been used mainly for an insect pest control. However, it is known that acute poisoning of the human body causes various symptoms such as dizziness, muscle weakness, dyspnea, skin irritation, and increased heart rate. Lately, eggs containing fipronil have been distributed and toxic problems are spreading around the world. In this study, we tried to develop analytical methods to evaluate the exposure of fipronil and fipronil sulfone in animal serum samples. The differences according to mobile phase and the results of liquid - liquid extraction and solid phase extraction pretreatment method were compared. Distilled water (A) and acetonitrile (B) were selected for the mobile phase, and the pretreatment method was determined by solid phase extraction. As a result of the method validation, the intra-day / inter-day accuracies were 82.2~114.1% and the precisions were less than 20%. The detection limit was 0.027 ng/ml for fipronil and 0.087 ng/ml for fipronil sulfone. The linearity obtained was satisfying, with a coefficient of determination (r²) higher than 0.99. The concentrations in some animal sera were determined using the methods of analysis for fipronil and fipronil sulfone in animal sera developed in this study. Using the method developed in this study, it could be used as an analytical method for human bio-monitoring of fipronil and fipronil sulfone as well as animal serum.

• The Korean Journal of Pesticide Science
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• v.4 no.1
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• pp.1-10
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• 2000

The purpose of this study is to establish the assessment techniques of hazardous chemicals by the development of analytical method of biological samples. In this study, we have developed an extraction method of nine pesticides used for rice paddy that resulted in high recovery from the spiked human urine by the liquid-liquid extraction with diethyl ether at pH 7.0. Calibration curve obtained from each pesticide standard using by gas chromatography/mass spectrometry/selected ion monitoring has shown good linearity and detection limits were the range of $0.4{\sim}2.0$ ng/mL in urine. As a biological monitoring, urine samples of local farmers exposed directly to nine pesticides in the field were collected and analyzed by GC/MS. Of the tested pesticides, metabolites of phenthoate assumed were identified by GC/MS analysis. No parent compound was detected.

• Analytical Science and Technology
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• v.26 no.1
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• pp.19-26
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• 2013

Gibberllic acid ($GA_3$) is one of gibberellins (GAs) that are a class of plant growth hormones that exert profound and diverse effects on plant growth and development. $GA_3$ is essentially non-UV absorbing and is difficult to assay by UV-detector. For effective extraction of gibberellic acid from fruits by using liquid-liquid extraction, optimized pH and extraction solvent were established. The selective and sensitive derivative of $GA_3$ for HPLC/UV-vis was derivatized using phenacyl bromide, and the experimental factors, including reaction time, reaction temperature and amount of derivatizing reagent and base were investigated for the effective synthesis. The derivatized $GA_3$ with phenacyl bromide was effectively analyzed by HPLC/UV-vis. The structure of derivatized $GA_3$ was confirmed by HPLC/ESI-MS. For apple, LOD and LOQ were 0.008 mg/kg and 0.027 mg/kg, respectively. For pear, LOD and LOQ were 0.003 mg/kg, 0.012 mg/kg, respectively. The established method can be applied to more effective analysis of $GA_3$ from plant and food.