• Title/Summary/Keyword: Liquid Liquid Extraction

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A Study on the Simultaneous Determination of Residual Zeranol, Zearalenone and Their Metabolites in Beef by Gas Chromatography/Mass Spectrometry (Gas Chromatography/Mass Spectrometry에 의한 우육 중의 잔류 Zeranol, Zearalenone 및 그 대사산물들의 동시 분석법에 대한 연구)

  • 이은섭;이용욱
    • Journal of Food Hygiene and Safety
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    • v.9 no.1
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    • pp.1-13
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    • 1994
  • A Simultaneous determination method was improved for the determination and confirmation of zeranol, zearalenone, as well as their isomers and metabolites, in beef. The analytes were extracted from tissue by CH3CN, hydrolyzed enzymatically(for glucuronide conjugates), cleaned up by a strong basic anion exchange resin combined with a liquid/liquid partitioning, derivatized using MSTFA and confirmed, quantified by GC/MS/SIM with a internal standard, zearalane. The results were as follows : (1) all the estrogens were separated on the GC/MS chromatogram under the extraction method and the chromatographic conditions improved, the retention times of zearalane-TMS2, zearalanone-TMS2, zearalenone-TMS2, zeranol-TMS3, taleranol-TMS3, and $\alpha$-zearalenol-TMS3, $\beta$-zearalenol-TMS3, were 18.49, 19.44, 19.63, 19.71, 19.79 and 19.99, 20.08 minutes, respectively. (2) The calibration curves of residual zeranol, zearalenone and their metabolites showed constantly linear(r=0.99) in the range of 5~20 ng. The minimum detection concentration of residual zeranol, zearalenone and their metabolites was 1 ppb. (3) The total average recovery of residual zeranol, zearalenone and their metabolites from spiked beef was 60.2%(CV=29.7%) at the 1 ppb and 63.5%(CV=26.5) at the 2 ppb, 72.9%(CV=18.2%) at the 4 ppb. (4) The preservation method for 6 estrogens was improved for the fast running time(21 min) and MSTFA was utilized for derivatizing 6 estrogens for improvement of recovery, for good resolution, for characteristic mass spectra unlike Jose's method and Tina's method. The utilization of zearalane as internal standard showed good quantification result for zeranol, zearalenone, as well as their isomers and metabolites, in beef.

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Simultaneous Quantification of Oleins (triolein, diolein and monoolein) in Mouse Feces using Liquid Chromatography-Electrospray Ionization/Mass Spectrometry

  • Lim, Jong-Hyun;Lee, Jeong-Ae;Jang, Yu-Ra;Chung, He-Sson;Lee, Won-Yong;Chung, Bong-Chul
    • Mass Spectrometry Letters
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    • v.3 no.3
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    • pp.68-73
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    • 2012
  • Fat malabsorption is an important cause of poor growth in infancy and childhood. Steatorrhea tests have been developed using various methods. Traditional measurements of stool fat, however, require large samples and it often takes as a week to complete the analysis. In this paper, a liquid chromatography-electrospray ionization/mass spectrometry (LC-ESI/MS) method was developed for simultaneous quantitative analysis of triacylglycerols, triolein, diolein and monoolein, in mouse feces. Moreover, the procedure was rapid, simple as well as compatible with LC-ESI/MS. Chloroform-isopropyl alcohol solution was used for fat-soluble sample extraction. After centrifugation and filtration, an analytical solution was prepared. Triolein, diolein and monoolein were separated using non-aqueous reversed-phase column with the mobile phase consisting of A (methanol) and B (acetone-isopropyl alcohol). The precision (% CV) and accuracy (% bias) of the assay were 3.8-14.7% and 85.2-114.9%, respectively. This method has been successfully applied to simultaneous determination of triolein, diolein and monoolein in feces from 30 mice. This method can therefore be applied to measure triacylglycerols in mouse feces accurately and precisely by LC-ESI/MS, thereby helping to predictive biomarker in fat malabsorption and diagnostic research.

A CLINICOSTATICAL STUDY OF JAW CYST BETWEEN 2001${\sim}$2005 (최근 5년간 구강악안면 낭종 환자에 대한 통계학적 검토)

  • Lim, So-Yeon;Yeo, Duck-Sung;Lee, Hyun-Jin;Kim, Hyun-Kyung;An, Kyung-Mi;Sohn, Dong-Seok
    • Journal of the Korean Association of Oral and Maxillofacial Surgeons
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    • v.32 no.6
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    • pp.588-593
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    • 2006
  • Cyst is pathologic disease develops in hard tissue as well as soft tissue, which is lined by epithelium filled with liquid, semi-liquid, or air. Origins and symptoms of the cyst are various according to region, and symptoms are malocclusion, diversion of root, tooth mobility, periapical swelling, discoloration and lesion expansion, because the odontogenic cysts begin in the numerous rests of odontogenic epithelium. But almost cysts produce no symptoms unless secondary infection occurs. Treatment of small cysts may include extraction, endodontic therapy, and apical surgery. Treatment of a large cysts usually involves surgical removal (enucleation), Marsupialization(a method of decompression) or combination of two before mentioned. Bone graft is done for helping of bone defect healing at the same time of enucleation This clinical research from January 2000 to December 2005, analyzed by the age, sex, classification, size, region, treatment method, whether or not of bone graft of cyst in the jaw in Daegu Catholic University Hospital.

Characteristic Study for Methyl-mercaptain Removal by an Essential Oil (식물추출물을 이용한 메틸멀캡탄 제거 특성 연구)

  • Park, Young-Gyu
    • KSBB Journal
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    • v.22 no.3
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    • pp.151-156
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    • 2007
  • Increasing public concerns over odors and air regulations necessitates the remediation of a wide range of odorous compounds for industrial purpose. Currently, wet scrubbing technique by neutralization using essential oils is utilized to treat methyl mercaptan odor. The chemical analysis is performed to analyze the composition of an essential oil by GC-MS. The objective of this study is to clarify the possibility of the neutralization of odors sprayed in the fixed bed and determine the removal efficiencies in the misty aerosol by different input odor concentration. It is found that methyl mercaptan is significantly removed in the wet scrubber, and their removal efficiency of methyl mercaptan is obtained by 98%.

Analysis of Penicillin Antibiotics in Aquatic Products (수산물 중 penicillin계열 항생제의 분석)

  • Bae, Jin-Han;Kim, Bo-Mi;Choi, Mi-Sun;Roh, Hye-Jin;Park, Mi-Jung
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.43 no.6
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    • pp.629-636
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    • 2010
  • A simple, rapid method for determining amoxicillin (AMO) and ampicillin (AMP) in aquatic products (flatfish, salmon, shrimp, tilapia, and yellow croaker) was evaluated. For quantification, the AMO and AMP ions at m/z 348.9 and 105.9, respectively, were selected. The limit of detection (LOD) and limit of quantification (LOQ) for detecting AMO were 0.09 and $0.25\;{\mu}g/L$, respectively. The respective values for AMP were 0.02 and $0.05\;{\mu}g/L$. After $100\;{\mu}g/L$ AMO treatment, the level decreased 10% after 7 days at $5^{\circ}C$, while it decreased 20% at $25^{\circ}C$. After 7 days, 94.9.100% of $100\;{\mu}g/L$ AMP remained after storage at $5^{\circ}C$, while 62.3.100% remained after storage at $25^{\circ}C$. Using the food code method, the recovery of AMO ranged from 64.1.92.0% and that of AMP from 44.8.86.2%. With a protein centrifugation method, the recovery of AMO ranged from 39.8.87.9% and that of AMP from 78.0.98.1%. With liquid-liquid extraction, the recovery of AMO ranged from 36.5.88.3% and that of AMP from 31.8.75.1%.

Isolation and Partial Characterization of Phytotoxic Mycotoxins Produced by Sclerotinia sp., a Potential Bioherbicide for the Control of White Clover(Trifoliorum repens)

  • Hong, Yeon-Kyu;Lee, Bong-Choon;Jung, Won-Kwon;Bae, Soon-Do;Park, Sung-Tae;Uhm, Jae-Youl
    • The Plant Pathology Journal
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    • v.20 no.1
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    • pp.52-57
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    • 2004
  • Sclerotinia sp. (isolate BWC98-105) causes stem blight and root rot in Leghum sp., and is presently being evaluated as a potential mycoherbicide for the control of Trifoliorium repens. Bioassays have shown that Sclerotinia sp. produces phytotoxic substance which is biologically active against T. repens. Two biologically active compounds, designated as compoundsI and II, were produced in vitro from the culture filtrate of BWC98-105 isolate Sclerotium sp. Compounds I and II were purified by means of liquid-liquid extraction and $C_{18}$ open column chromatography (300 ${\times}$ 30 mm, i.d). To determine the purity, the purified compounds were analyzed by RP-HPLC. The analytical RP-HPLC column was a TOSOH ODS-120T (150 ${\times}$ 4.6 mm i.d, Japan), of which the flow rate was set at 0.7 mL/min using the linear gradient solvent system initiated with 15 % methanol to 85 % methanol for 50 min with monitoring at 254 nm. Under these RP-HPLC conditions, compounds I and II eluted at 3.49 and 4.13 min, respectively. Compound II was found to be most potent and host specific. However, compound I had a unique antibiotic activity against phytopathogenic bacteria like bacterial leaf blight (Xanthomonas oryzae) on rice, where it played a less important role in producing toxicity on T. repens. No toxin activity was detected in the water fraction after partitioning with several organic solvents. However, toxin activity was detected in the ethyl acetate and butanol fractions. In the leaf bioassay using compound II, the disease first appeared within 4-5 h as water soaked rot, which subsequently developed into well-defined blight affecting the whole plant.

Determination and survey of tetracyclines residue in honey by high performance liquid chromatography (액체크로마토그래피를 이용한 벌꿀 중 테트라싸이클린계 항생물질의 정량분석 및 잔류조사)

  • Lee Sung-Mo;Park Eun-Jeong;Hong Jee-Young;Kim Jung-Im;Lee Jung-Goo;Hwang Hyun-Soon;Kim Yong-Hee
    • Korean Journal of Veterinary Service
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    • v.28 no.3
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    • pp.203-213
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    • 2005
  • Oxytetracycline, tetracycline, chlortetracycline and doxycycline in honey were separated by solid phase extraction (SPE) and determined with high performance liquid chromatography (HPLC) with UV/Visible detector. Analysis was carried out using following conditions: XTerra $C_8$ column $(3.9\times150mm\;i.d. 5{\mu}m)$, mobile phase composed of 0.01M oxalic acid : methanol : acetonitrile (820 : 80 : 100, v/v/v), isocratic pump at a flow rate of 0.9 ml/min. and $50{\mu}l$ of injection volume, UV/Visible detector with wavelength of 360nm. The calibration curves of four tetracyclines showed linearity $(\gamma^2>0.999)$ at concentration range of $100\~1,000 ng/ml$. The recoveries in fortified honey represented more than $70\%$ with low coefficient of variation $(<10\%)$ for concentration range of four tetracyclines. The detection limits for oxytetracycline, tetracycline, chlortetracycline and doxycycline were 13.8, 14.6, 26.2 and 24.9ng/g in acacia honey. respectively. We also monitored tetracyclines residue in domestic honey [n : 38, acacia (20), wild flower (18) ] and foreign honey [n=22, legally distributed (13), illegally distributed (9)] using modified Charm II screening and HPLC confirmation methods. Seven of the 60 samples $(11.7\%)$ were suspect positive using modified Charm II screening test. Chlortetracycline residue was found in one foreign honey (illegally distributed) tested at concentrations of 0.22 ppm. Conclusively, for more effective control of tetracyclines used in beekeeping should be further survey for residues in honey and also national guidelines (maximum residue limit : MRL) and methods should be obligatory.

Development of Solid/Liquid Separation Technique for Krill (Eupausia superba) (남극 크릴새우의 고액분리 기술개발)

  • Oh, I.H.;Jang, C.H.;Kim, W.G.;Yang, S.Y.
    • Journal of Animal Environmental Science
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    • v.17 no.1
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    • pp.33-38
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    • 2011
  • Economic development involves increase in life expectancy as well as human health care. Consequently, demand for fish meal and fish oil is rapidly growing. In particular, Krill (Eupausia superba) oil product is in high demand due to its rich unsaturated-fatty acid, and thus stable supplies are necessary in the krill oil market. It is required for captured krills to be immediately frozen and stored during ship transport, since proteins of the krill are quickly denatured in natural temperature condition. However, the transportation cost has been sharply increased, which encourages researchers to involve in studies for development of efficient oil extraction process. In this study, a solid/liquid separation technique on boat for the krill oil was developed through triple separation tests using only a separator or using either brush or crusher prior to the separator. The separation tests revealed that the efficiency were 46.2, 60.2 and 60.4 % by the separator, combination with brush, and combination with crusher, respectively. In addition, it was found that byproduct, extracted cake, derived from the separation process could be used as a feed stuff. These results suggest that smashing using the brush or crusher prior to the separator is more efficient than using only the separator.

Simple and Sensitive Liquid Chromatography Electrospray Ionization Mass Spectrometry Method for Determination of Glycoalkaloids in Potato (Solanum tuberosum L.)

  • Kim, Jae-Kwang;Bae, Shin-Cheol;Baek, Hyung-Jin;Seo, Hyo-Won;Ryu, Tae-Hun;Kim, Jung-Bong;Won, So-Youn;Sohn, Soo-In;Kim, Dong-Hern;Kim, Sun-Ju;Cho, Myoung-Rae
    • Food Science and Biotechnology
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    • v.18 no.1
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    • pp.113-117
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    • 2009
  • A method was developed using enhanced liquid chromatography coupled with electrospray ionization mass spectrometry for the analysis and quantitation of 2 main potato glycoalkaloids, $\alpha$-chaconine, and $\alpha$-solanine, without any pre-concentration or derivatisation steps. Calibration curves generated by this technique exhibited a linear dynamic range from 0.025 to $50{\mu}g/mL$ and from 0.05 to $50{\mu}g/mL$ for $\alpha$-chaconine and $\alpha$-solanine, respectively. Matrix effects were evaluated by comparing calibration curves measured in matrix-matched and solvent-based systems. Ion suppression due to matrix effects was weak and extraction recoveries of 88 to 114% were obtained in different sample matrices spiked with analyte concentrations ranging from 15 to $35{\mu}g/mL$. Potatoes that had been genetically modified to tolerate glufosinate contained the same glycoalkaloid levels as their non-transgenic counterpart. We suggest complementing compositional comparison assessment strategy by validating quantitative analytical methods for the toxic glycoalkaloids in potato plants.

Airborne Suspended Particulates Concentration and Cancer Risk Assessment of Polycyclic organic matter in Seoul (서울시 대기부유분진의 농도와 다환방향족 유기물질에 의한 발암 위해성)

  • Park, Seoung-Eun;Chung, Young
    • Journal of Korean Society for Atmospheric Environment
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    • v.8 no.4
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    • pp.247-256
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    • 1992
  • Airborne suspended particulates were collected at Shinchon by a high volume cascade impactor from Sep. 1990 to Aug. 1991. Organic matter was extracted from particulates and fractionated by liquid-liquid extraction and thin layer chromatography. Substances in the PAHs and nitroarenes'subfraction of neutral fraction were determined by capillary gas chromatography. Based on unit risk estimates by multi-stage model of benzo[a]pyrene and the results of exposure estimates, cancer risk was assessed. The annual average concentration of total suspended particulates was 201.77g/$m^3$. The percentage of fine particulates was 57.40. The concentration of total suspended particulates showed seasonal variations and was high in winter and spring. The average concentration of extractable organic matter was 8.12g/$m^3$. In all, 21 PAHs were identified and quantified. The annual concentration of fluoranthene was 2.38ng/$m^3$, and that was the highest value of all PAHs. A carcinogenic compound, benzo[a]pyrene, was at a concentration of 1.84ng/$m^3$. All the 10 nitroarenes were also identified and quantified. The major nitroarene in the Shinchon area was 2,7-dinitrofluorene. The annual concentration of 1-nitropyrene was 1.56ng/$m^3$. Concentrations of PAHs and nitroarenes were high in winter and low in summer. The life time excess risk estimates of benzo[a]pyrene was calculated as 0.96 persons/a million population in this experiment. In the rank of relative potenties, carcinogenic effects of the other PAHs were calculated as 0.004-0.108 persons/a million population.

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