• Title/Summary/Keyword: Liquid Liquid Extraction

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Quantitative Analysis of Microcystins, Cyanobacterial Toxins in Soyang Lake (소양호에서 남조류 독소, 마이크로시틴의 정량 분석)

  • Lee, Jeong Ae;Lee, So Yeong;Pyo, Dong Jin
    • Journal of the Korean Chemical Society
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    • v.46 no.6
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    • pp.535-540
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    • 2002
  • It is very difficult to analyze the microcystins, cyanobacterial toxins quantitatively since it exists in a trace level in lakes. In this paper, two different analytical methods were tried to analyze the microcystins, cyanobacterial toxins quantitatively in water samples collected in Soyang lake. The first method was solid phase extraction method fol-lowed by High Performance Liquid Chromatography(HPLC), and the second method was Enzyme-Linked Immu-nosorbent Assay(ELISA) using the monoclonal antibody of microcystin.

Mobile Phase Compositions for Ceramide III by Normal Phase High Performance Liquid Chromatography

  • Hong, Seung-Pyo;Lee, Chong-Ho;Kim, Se-Kyung;Yun, Hyun-Shik;Lee, Jung-Heon;Row, Kyung-Ho
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.9 no.1
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    • pp.47-51
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    • 2004
  • Ceramide III was prepared by the cultivation of Saccharomyces cerevisiae. Ceramide III was partitioned from the cell extracts by solvent extraction and analyzed by Normal Phase High Performance Liquid Chromatography (NP-HPLC) using Evaporative Light Scattering Detector (ELSD). We experimentally determined the mobile phase composition to separate ceramide III with NP-HPLC. Three binary mobile phases of n-hexane/ethanol, n-hexane/lsoprophyl Alcohol(IPA) and n-hexane/n-butanol and one ternary mobile phase of n-hexane/IPA/methanol were demonstrated. For the binary mobile phase of n-hexane/ethanol, the first mobile phase composition, 95/5(v/v), was step-increased to 72/23(v/v) at 3 min. In the binary mobile phase, the retention time of ceramide III was 7.87min, while it was 4.11 min respectively in the ternary system, where the mobile phase composition of n-hexane/IPA/methanol, 85/7/8(v/v/v), was step-increased to 75/10/15(v/v/v) at 3 min. However, in the ternary mobile phase, the more peak area of ceramide III was observed.

Determination of amitraz by high-performance Liquid chromatography with photodiode array detection and method validation (HPLC-PDA를 이용한 Amitraz의 분석법 확립 및 검증)

  • Yun, Hyeong-Jun;Yun, So-Mi;Lee, Myoung-Heon;Son, Seong-Wan
    • Korean Journal of Veterinary Research
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    • v.48 no.1
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    • pp.33-38
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    • 2008
  • In veterinary medicine amitraz has been used as an insecticide to eliminates mites, lice, and ticks in dogs, cats, goats, swine and cattle. The objective of present study was to developed an analytical method using one-step extraction and determination of the amitraz in veterinary drugs by liquid chromatography (LC). The amitraz was analyzed by LC equipped with Waters XTerra RP18 ($4.8{\times}250mm;\;5{\mu}m;\;Waters,\;USA$) analytical column, using 75% acetonitrile (acetonitrile/D.W; 75/25) at 1.0 ml/ min. The UV-VIS detection of amitraz was made at 290 nm. Calibration graphs were linear with very good correlation coefficients ($r^2>0.9999$) from $80{\sim}120{\mu}g/ml$. The limit of detection was $0.09{\mu}g/ml $ and limit of quantification was $0.27{\mu}g/ml $. The method showed good intra-day precision (CV 0.05~0.09%) and inter-day precision (CV 0.06~0.18%).

Synthesis and Properties of New Polymeric Photostabilizers Containing HALS Groups (HALS 그룹을 가진 새로운 고분자형 자외선 안정제의 합성 및 특성)

  • 김한식;채규호
    • Polymer(Korea)
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    • v.25 no.5
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    • pp.625-634
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    • 2001
  • New polymeric photostabilizers containing hindered amine light stabilizer (HALS) were prepared by the reaction of liquid polyisoprene rubber grafted maleic anhydride (MAH) and 2,2,5,6-tetramethyl-4-piperidinol (TMPO). Their chemical composition and physical properties were characterized by titration, GPC and TGA analysis. The effects of polymeric HALS on the photooxidation of the styrene-butadiene rubber were studied from the UV, IR spectral changes, and photo-crosslinking was examined by the measurement of the insoluble fraction. The photooxidation of SBR upon irradiation was inhibited by addition of the new polymeric HALS. The extraction resistance of new polymeric photostabilizer was much better than that of the low molecular weight compound which is prepared by the reaction of MAH and TMPO. The new polymeric HALS ate fairly compatible with the SBR.

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Identification of Irradiation-induced Volatile Flavor Compounds in Irradiated Pork Meats (방사선 조사 돼지고기에서 휘발성 조사물질의 구명)

  • Cha, Yong-Jun;Kim, Hun;Cho, Woo-Jin;Jung, Yeon-Jung;Byun, Myung-Woo;Yoo, Young-Jae
    • Journal of Life Science
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    • v.11 no.1
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    • pp.35-42
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    • 2001
  • Irradiation-induced volatile flavor compounds in irradiated (0, 1, 3, 5, 10 kGy) pork meats were analyzed by liquid liquid continuous extraction (LLCE) and gas chromatography/mass spectrometry (GC/MS) methods. One hundred nine volatile compounds were detected in irradiated pork meats. These compounds were mainly composed of hydrocarbons (42 compounds), aromatic compounds (39), aldehydes(9), ketones(5) and miscellaneous compounds (14). Among these, three volatile compounds, such as decene, 1,2,3,4,-tetrahydro-6-methylnaphthalene and 1,2,3,4-tetrahydro-dimethylnaphthalene were selected as irradiation-induced compounds comparing with irradiation dosages in irradiated pork meats. By the high correlation coefficient with the increment of irradiation dose, however, decene (r=0.93) was considered as marker compound for detecting irradiation dosage in fresh pork meats.

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Matrix Solid-Phase Dispersion (MSPD) Isolation and Liquid Chromatographic Determination of Residual Furazolidone in Eggs (MSPD 전처리법과 HPLC를 이용한 Furazolidone의 계란내 잔류분석)

  • 서계원;이재일;이채용;이정치
    • Journal of Food Hygiene and Safety
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    • v.18 no.2
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    • pp.43-50
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    • 2003
  • A liquid chromatographic method, using matrix solid-phase dispersion (MSPD) is developed for the extraction of residual furazolidone in chicken eggs. Blank or fortified egg samples (0.5 g) were blended with Octadecylsilyl (Bulk $C_{18}$, 40${\mu}{\textrm}{m}$, 18%. load, endcapped. 2 g) derivatized silica. After homogenization, $C_{18}$/egg and Na$_2$S $O_4$matrix were transferred to a column made of 10 ml glass syringe and filter paper and compressed 4.0∼4.5 ml volume. The column was washed with 8 ml of hexane and dried under $N_2$ gas. Furazolidone was eluted with acetonitrile (8 ml) under gravity. The eluate containing furazolidone was free from interfering compounds when analyzed by HPLC with UV detection (365 nm, photodiode array). Calibration curves were linear (r = 0.99985) and inter- (1.47%) and intra-assay (5.29%) variabilities for the concentration range examined (7.8∼497 ng/g of eggs, 20 ${mu}ell$ injection volume) were indicative of an acceptable methodology for the analysis of furazolidone. Average recovery of furazolidone added to egg was 96.2%. The limit of detection for the proposed method was 1 ng/g for furazolidone. The method using MSPD is proposed as an alternative assay to the classical method which involves the use of large volumes of a harmful solvent and requires a long tedious separation and clean-up processes prior to its determination.

Investigation of Domoic acid in Shellfish Collected from Korean Fish Retail Outlets

  • Choi, Kyu-Duck;Lee, Jong-Soo;Lee, Jong-Ok;Oh, Keum-Soon;Shin, Il-Shik
    • Food Science and Biotechnology
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    • v.18 no.4
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    • pp.842-848
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    • 2009
  • The purpose of this study was to determine the extent of domoic acid (DA) a potent neurotoxin, responsible for the syndrome amnesic shellfish poisoning (ASP) contamination of various species of bivalve shellfish purchased from fish market in Korea and the implications for food safety. Liquid chromatography (LC) methods were applied to quantify DA in shellfish after sample clean-up using solid-phase extraction (SPE) with strong anion exchange (SAX) cartridges. Toxin detection was achieved using photodiode array ultraviolet (LC-UV) and electrospray ionization-mass (LC-ESI-MS). DA was identified in 4 bivalve shellfishes of 872 shellfishes collected from March, 2006 to October, 2007 in Korea. DA amount of 3 surf clams (Mactra veneriformis) collected at Seoul, Daejeon, and Daegu were 4.13, 1.99, and 1.94 mg/kg, respectively. DA amount of 1 pink butterfly shell (Peronidia venulosa) collected at Seoul was 3.02 mg DA/kg. The amounts of DA that were present in 4 bivalve shellfishes were within EU guideline limits for sale of shellfish (20 mg DA/kg).

Determination of Simultaneous Analytical Method of Residual Pesticides by Gas Chromatography (기체크로마토그래피를 이용한 잔류농약 동시다성분 분석법)

  • Choi, Won-Jo;Choi, Gye-Sun;Lee, Hee-Jung;Won, Young-Jun;Park, Heung-Jai;Kim, Woo-Seong
    • Journal of Environmental Science International
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    • v.18 no.12
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    • pp.1369-1381
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    • 2009
  • The simultaneous determination of residual pesticides was developed using a gas chromatography. In this study, a simple and reliable methodology was improved to detect 175 kinds of residual pesticides by a liquid-liquid extraction procedure, followed by chromatographic analysis by gas chromatography. The 175 kinds of residual pesticides was classified into 4 groups according to the chemical structure, column type, resolution and sensitivity. The soybean sample selected for recovery experiment was not detected any pesticides. The recovery rates were ranged from 70.6% to 119.7% in most pesticides. The relative standard deviation (RSD 0.3~5.6%) was lower than 5.6% in all cases. The limits of detection (LOD) was lower than the maximum residue levels established by Korean legislations. The method has been successfully applied to the analysis of approximately 130 real samples.

Identification of Character-impact Aroma Compounds and Comparisons of Sensory Attributes of Traditional Korean Medicinal Rice Wines Brewed with Functional Herbal Powders or Extracts

  • Lee, Gyu-Hee;Shin, Young;Chang, Yeong-Il;Jeong, Jae-Hong;Chang, Kyu-Seob;O, Man-Jin
    • Preventive Nutrition and Food Science
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    • v.7 no.4
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    • pp.405-410
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    • 2002
  • Rice wine was prepared with medicinal plants or plant extracts to obtain a value added nutritious alcoholic tonics. Powders of ten medicinal plants (PTM) or aqueous extracts prepared from them (ATM) were added during the initial stage of fermentation. Aroma compounds of rice wine (control) and wines containing PTM or ATM were isolated by liquid-liquid continuous solvent extraction (LLCSE) and analyzed by gas chromatography-olfactometry and aroma extract dilution analysis (AEDA). Desirable aroma compounds: acetaldehyde (sweet, ethereal), benzaldehyde (sweet, fragrant), ethyl acetate (sweet) and ethyl octanoate (sweet, ethanolic) had the highest log$_3$-flavor dilution (FD) factors in ATM. Results of sensory evaluation demonstrated that intensities of undesirable aroma attributes, such as koji and yeasty notes in control, and raw medicinal herb notes in PTM, were lowest in wine with ATM. Wines made with ATM had the most attractive aroma attributes among the three different traditional Korean medicinal wines.

Identification and Characterization of Homoharringtonine from Cephalotaxus koreana

  • Kim, Byung-Sik;Kim, Jin-Hyun
    • 한국생물공학회:학술대회논문집
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    • 2005.10a
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    • pp.566-569
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    • 2005
  • A novel purification method was developed for producing homoharringtonine from Cephalotaxus koreana, to guarantee high purity and yield. Our simple, efficient procedure for isolating and purifying homoharringtonine from C. koreanabiomass consisted of solvent extraction, synthetic adsorbent treatment, low-pressure chromatography, followed by high performance liquid chromatography (HPLC). The use of active clay treatment and silica gel low-pressure chromatography in the pre-purification process allowed for the rapid, efficient separation of homoharringtonine from interfering compounds and dramatically increased the yield and purity of crude homoharringtonine for high-performance liquid chromatography (HPLC) purification steps compared with alternative processes. Homoharringtonine could be obtained simply with high yield and purity from biomass using this purification method, while minimizing solvent use and the scale and complexity of HPLC operations for homoharringtonine purification. Purified homoharringtonine was identified and characterized.

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