• Title/Summary/Keyword: extraction residue

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Simultaneous Determination of Sulfonamides in Porcine and Chicken Muscle Using High Performance Liquid Chromatography with Ultraviolet Detector

  • Shim, You-Sin;Shin, Dong-Bin;Cho, Yong-Sun;Choi, Yun-Hee;Lee, Sang-Hee
    • Food Science and Biotechnology
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    • v.18 no.6
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    • pp.1430-1434
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    • 2009
  • The present study used the liquid extraction pretreatment method and developed a liquid chromatographyultraviolet detector (LC-UV) for the simultaneous determination of 14 sulfonamides (SAs) residues in porcine and chicken muscle. Linearity within a range of $50-150\;{\mu}g/kg$ was obtained with the correlation coefficient ($r^2$) of 0.9673-0.9997. The mean recovery of SAs was 55.9-109.7% (relative standard deviations; RSDs 1.7-17.3%) in porcine muscle and 52.8-112.4% (RSDs 2.3-16.9%) in chicken muscle. The limits of detection (LODs) and limits of quantification (LOQs) were 2-32 and $7-96\;{\mu}g/kg$ in porcine muscle, and 4-32 and $13-97\;{\mu}g/kg$ in chicken muscle, respectively. These values were lower than the maximum residue limits (MRLs) established by the European Union. The sum of all SAs residues present should be less than $100\;{\mu}g/kg$.

Postmortem Distribution of Methidathion in Human Specimens of a Acute Poisoning (Methidathion 중독사에 의한 사후혈액 및 조직중 분포)

  • 이종숙;이재신;최동기;양희진;이상기;구기서;유영찬
    • YAKHAK HOEJI
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    • v.46 no.2
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    • pp.93-97
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    • 2002
  • Methidathion is one of the organophosphorus pesticides commonly used for stamping out harmful pests in farming areas. This paper presents a fatality due to methidathion intoxication and describes the distribution of methidathion in postmortem blood and tissues obtained at autopsy. Qualitative identification of methidathion was achieved by TLC, GC and GC/MS, and quantitative analysis was performed by GC with thermionic specific detector (TSD). The analytes in postmortem specimens were extracted by liquid-liquid extraction (LLE) with ethylether. After the ethylether layer was evaporated, the residue was partitioned into hexane and acetonitrile, and the acetonitrile layer was used for analysis. Tissue specimens were homogenized with 4% perchloric acid and applied for LLE. After extraction, the extracts were reconstituted 100 $\mu\textrm{g}$ pyraclofos (IS, 100 $\mu\textrm{g}$/ml in methanol) for GC and GC/MS analysis. On analysis of postmortem specimens, methidathion was identified and quantitated. The methidathion concentrations were 2.0 $\mu$l/ml in blood, 24.4 $\mu\textrm{g}$/g in liver, 13.9 $\mu\textrm{g}$/g in lung, 21.8 $\mu\textrm{g}$/g in kidney, respectively.

Studies on Volatile Flavor Compounds of Soy Sauce Residue (간장박의 휘발성 향기성분에 관한 연구)

  • Cha, Yong-Jun;Wang, Wenfeng;Cha, Ha-Ram
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.12
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    • pp.1755-1761
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    • 2016
  • Volatile flavor compounds in soy sauce residue (SSR) and acid hydrolysate of SSR (AHSSR) were analyzed by solid phase micro extraction (SPME)/gas chromatography (GC)/mass spectrometry (MSD) methods. A total of 79 compounds were detected in samples (66 SSR and 60 AHSSR). Quantitatively, alcohols (433.37 ng/g), aldehydes (273.01 ng/g), esters (236.80 ng/g), and aromatic hydrocarbons (180.66 ng/g) were dominant in the volatiles of SSR, whereas furans (249.27 ng/g) were only dominant in AHSSR (P<0.05). Among these, four esters, 3-methylbutyl acetate (banana/pear-like), ethyl 3-methyl butanoate (fruity), ethylbenzene acetate (wine-like), and ethyl 3-methyl butanoate (apple-like), three alcohols, 3-methyl-1-butanol (fruity/whisky-like), 2-phenylethanol (floral/sweet), and 1-octen-3-ol (mushroom-like), four aldehydes, (E)-2-phenyl-2-butenal (chocolate-like), benzaldehyde (almond-like), 3-methylbutanal (malty), and 2-phenylacetaldehyde (floral), four aromatic hydrocarbons, 4-ethyl-2-methoxyphenol (smoky/soy sauce-like), 4-ethylphenol (medicine-like), 4-vinyl-2-methoxyphenol (woody), and phenol (woody), and two furans, furfural (almond-like) and 4-hydroxy-2,5-dimethyl-3(2H)-furanone (caramel-like), were major compounds in SSR, whereas seven compounds, including furfural, 5-methylfurfural (almond-like), 3-methyl-1-butanol, 2-phenylethanol, 4-ethyl-2-methoxyphenol, 3-methylbutanal, and benzaldehyde were major compounds in AHSSR.

Tissue Distribution after dipping administration of Oxytetracycline and Tetracycline in Olive flounder (Paralichthys olivaceus), Rockfish (Sebastes schlegeli), and Red sea bream (Pagrus major) (Oxytetracycline과 Tetracycline의 약욕에 따른 양식어류 (넙치, 조피볼락, 참돔)의 조직내 잔류량의 변화)

  • Lee, Hu-Jang;Kim, Suk;Ha, Ji-Young;Kang, Seok-Jung;Jung, Won-Cheol;Chung, Hee-Sik;Heo, Sung-Hyek;Shin, Yong-Woon;Kim, Kyoung-Won;Kim, Dae-Geun
    • Journal of fish pathology
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    • v.19 no.2
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    • pp.155-164
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    • 2006
  • Tissue distribution and residue depletion of oxytetracycline (OTC) and tetracycline (TC) following dipping administration were evaluated in olive flounder (Paralichthys olivaceus), rockfish (Sebastes schlegeli), and red sea bream (Pagrus major) under field conditions. Fishes were held in floating cages placed in sea water and fed a commercial diet for 15 days to acclimate to a new surrounding. Fishes were dipped in OTC 50 g/ton water for 30min and TC 18 g/ton water for 5 hours. Blood and muscle were sampled from fishes on 0th, 1th, 2th, 3th, and 5th day after administration. After solid-phase extraction, OTC and TC analyses were carried out by HPLC. The recovery rate of OTC in serum and muscle samples was 71-77% and 78-84%, respectively. Also, the recovery rate of TC in serum and muscle samples was 70-79% and 73-78%, respectively. The results of recovery rate were similar to previous studies reported. At the termination of dipping administration of OTC and TC, residue concentration in muscle samples of rockfish was significantly higher than those of olive flounder and red sea bream. At day 5, residue concentrations of all samples were believed to decrease to lower than 0.05 mg/kg, the detection limit. The present study showed that residue concentrations of OTC and TC decreased to below 0.05 mg/kg after treatment 5th day, faster than the established withdrawal period. The tissue reside depletion time of dipping administration of OTC and TC seems to be shorter than those of oral or parenteral administration.

Mechanical and Barrier Properties of Soybean Curd Residue Protein Films (비지 단백질로 제조한 가식성필름의 기계적 및 물질투과특성)

  • Cho, Seung-Yong;Park, Jang-Woo;Rhee, Chul
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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    • v.5 no.2
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    • pp.9-16
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    • 1999
  • Edible films were prepared from proteins extracted from soybean curd residue by alkaline extraction and isoelectric precipitation. Effects of film forming solution pH and plasticizers on mechanical and barrier properties of edible films were studied. films were formed within pH $7{\sim}11$ with tensile strength (TS) of $2.9{\sim}3.3$ MPa. Films produced under pH 10 had the highest TS and Elongation (E) (3.3 MPa and 60.1%) but no significant difference was observed among water vapor permeabilities (WVP) of film. Glycerol, sorbitol and its mixture (1:1, w/w) were added as plasticizers. The concentration and mixing ratio of plasticizers also affected the TS, E and WVP of films. TS of films decreased from 15.0 MPa to 2.9 MPa as plasticizer concentration increased from 0.4 to 0.8 g plasticizer/g protein. At a plasticizer concentration, the highest TS was observed when sorbitol was used whereas the highest E was measured when mixture of glycerol and sorbitol was used as plasticizer WVP of films increased as the plasticizer concentration increased. Films plasticized with glycerol showed the highest WVP among the films with the same plasticizer concentrations. Edible films prepared from soybean curd residue protein showed very low oxygen permeabilities ($29.5{\sim}61.1aL{\cdot}m/m^2{\cdot}s{\cdot}Pa$) and oil resistance at all plasticizer concentration level tested.

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Analysis of Propylen Chlorohydrin in Hydroxypropyl Distarch Phosphate by Accelerated Solvent Extractor (ASE) (가속화용매추출기를 이용한 히드록시프로필인산이전분의 프로필렌클로로히드린 분석방법에 관한 연구)

  • Lee, Myung-Ja;Sin, Yeong-Min;Jeong, Eui-Han;Choi, Tae-Jin;Chung, Sook-Hyun;An, Won-Gun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.31 no.4
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    • pp.604-608
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    • 2002
  • Accelerated solvent extraction (ASE) was used for a rapid and simple extraction of propylenchlorohydrin (PCH) residue in hydroxylpropyl modified starch. The effects of temperature, pressure and extraction solvent on the extraction efficiency were investigated to find the optimal condition of ASE. The optimal conditions for PCH extraction in hydroxylpropyl modified starch were static time of 50 min, purge time of 300 sec, heating time of 5min, temperature of 12$0^{\circ}C$, pressure of 2500 psi, flush (%) with 100 volumes, and ethylacetate as an extraction solvent. The recovery (96.1%) of this method was higher than that (76.4%) of Code of Food Additive. Therefore, the ASE was a good method in both aspects of efficiency and effectiveness.

Studies on Pretreatment for Analysis of Pesticides by Using HPLC and GC (HPLC 및 GC에 의한 농약분석에서 전처리에 대한 연구)

  • Oh, Bo Young;Bae, Jun Hyun;Kang, Jun Gil;Kim, Youn Doo
    • Journal of the Korean Chemical Society
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    • v.43 no.6
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    • pp.663-669
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    • 1999
  • For determination of separated pesticides by using GC and HPLC, liquid-liquid extraction(LLE) and solid phase extraction(SPE) have been carried out to separate and concentrate the organophophorous pesticides such as Diazinon, Fenitrothion, Phosmet, Phosalon and EPN in environmental water samples. ln determination of pesticides by HPLC/UV, SPE has resulted in higher recovery and more precision than LLE, while in determination of pesticides by GC/FPD, vice versa. HPLC/UV after the pretreatment process of sample by solid phase extraction (SPE-HPLC/UV) has suggested the possibility of determination of pesticides ppb level. ln comparison of detection limit, both SPE-HPLC/UV and LLE-GC/FPD are reasonably suitable for analysis of residue pesticides. ln the respect of the rapidity and the solvent required, SPE-HPLC/UV method has proven to be superior to LLE-GC/FPD.

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Rapid Analysis of Tetraconazole Residues in Fruits and Vegetables using Ethyl Acetate Extraction and Gas Chromatography-tandem Mass Spectrometry

  • Xu, Jun;Dong, Fengshou;Liu, Xingang;Li, Jing;Li, Yuanbo;Shan, Weili;Zheng, Yongquan
    • Bulletin of the Korean Chemical Society
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    • v.32 no.12
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    • pp.4265-4269
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    • 2011
  • A method based on ethyl acetate extraction and gas chromatography with tandem mass spectrometry was developed for determining tetraconazole residues in fruits and vegetables. A 10 g homogenized sample was mixed with 10 mL ethyl acetate, shaken vigorously for 3 min, stored at $-20^{\circ}C$ for 15 min, and then vortexed vigorously for 1 min; 1 g NaCl and 4 g anhydrous $MgSO_4$ were added. The clean-up was carried out by applying dispersive solid-phase with 150 mg $MgSO_4$and 50 mg primary secondary amine. Three precursor product ion transitions for tetraconazole were measured and evaluated to provide the maximum degree of confidence. Average recoveries in fruits and vegetables at three levels (0.005, 0.05 and 0.5 mg/kg) ranged from 85.53% to 110.66% with relative standard deviations ($RSD_r$) from 1.3% to 17.5%. The LODs ranged from 0.002 to 0.004 ${\mu}g$/kg, and LOQs ranged from 0.006 to 0.012 ${\mu}g$/kg. This method was also applied to determine tetraconazole residue in cucumber dissipation experiment under field conditions. The half-lives of tetraconazole in cucumber were in the range of 2.1-3.1 days.

A New Cyclophilin Inhibitor from Ganoderma lucidum: Purification and Characterization

  • Lim, Jin-Ik;Jeong, Ki-Chul;Kang, In-Sug;Kim, Soo-Ja
    • Bulletin of the Korean Chemical Society
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    • v.25 no.7
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    • pp.1055-1060
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    • 2004
  • A new inhibitor for peptidylprolyl cis-trans isomerase (PPIase) has been isolated from Ganoderma lucidum and purified to homogeneous state by organic solvent extraction. The purified PPIase inhibitor (GPI) is assumed to be a membrane-associated glycoprotein. GPI inhibits specifically the bovine brain PPIase, a cyclophilin, and has no effect on the FKBP activity. The results of our chemical modification study of GPI indicate the presence of Lys residue(s) at or near its binding site. Like CsA-cyclophilin complex, GPI-bovine brain PPIase complex strongly inhibits the calcineurin activity in vitro, suggesting the possible involvement of GPI in immunomodulating pathway by the formation of PPIase-inhibitor-calcineurin complex.

Mutagenicity of Diesel-Exhaust Particulates

  • Yoo, Young S.
    • Journal of Korean Society for Atmospheric Environment
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    • v.10 no.E
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    • pp.325-331
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    • 1994
  • Organic extracts of diesel- exhaust particulates were analyzed for mutagenicity using Ames Salmonella typhimurium assay system. An experimental diesel microbus used was drived on the chassis dynamometer according to CVS-75 mode. The samples were taken from the mixed gases in a dilution tunnel. With a high-volume air sampler equipped with double filter holders, particulate matters were collected on a teflon-coated glass fiber filter placed behind a activated carbon filter. After ultrasonic extraction with benzene- ethanol and evaporation to dryness, the residue was dissolved in dimethylsulfoxide. Each sample was tested toward 2 strains, TA100 and TA98 by the pre-incubation method in the absence and presence of S-9mix. Average concentration of diesel- exhaust particulates was about 116.6mg/m$^3$, and 44.1~62.2 % to the total weight of particulates, consisted of organic matters. The mutagenicities of diesel- exhaust particulate organic matters were 4,512 and 2,205 revertants/m$^3$ toward TA100 without and with S-9mix, respectively. Those toward TA98 were 13,367 and 3,715 revertants/m$^3$, respectively.

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