• Title/Summary/Keyword: extraction residue

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Solid-Phase Extraction of Sulfamerazine from Shrimp Residue and Determination by Reversed Phase High Performance Liquid Chromatography

  • Jang, Won-Cheoul;Heo, Gang-Joon
    • Toxicological Research
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    • v.12 no.2
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    • pp.163-169
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    • 1996
  • The focus of this study was to investigate the suitable analytical methods for measurement of sulfamerazine and its metabolite in shrimp hepatopancreas and tail tissue, in addition to the methods for the optimization of solid-phase extraction cartridge conditions and the elucidation of sulfamerazine concentrations in aqueous buffer using HPLC with UV and EC detectors. Compared with UV detector the EC detector appears to be 10 times more sensitive than that of the UV detector. After the shrimp was exposed to 10 ppm sulfamerazine, the accumulation levels of sulfamerazine and its metabolite in tail tissue, which is edible portion, were considerably lower than 0.1 ppm. The data indicate that sulfamerazine continues to be a candidate for use at levels of sulfamerazine concentration used in aquaculture of shrimp.

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Extraction of proteins from soymilk residue using the enzymes from Bacillus subtilis (납두균 효소를 이용한 두유단백질의 용출)

  • Lee, Snag-Min;Kim, Ze-Uook
    • Applied Biological Chemistry
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    • v.33 no.4
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    • pp.282-286
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    • 1990
  • To extract insoluble proteins of soymilk residue by microorganism the soymilk residue was treated with crude enzyme solution from Bacillus subtilis IAM 1071 natto. Optimum conditions of pH, temperature, and digestion time were determined, and amino acid composition of the extract was obtained at $45^{\circ}C$. Under optimum conditions, the extractability with natto reached to 65% in 15hrs. The contents of essential amino acids of extract were high and specially, S-containing amino acids including methonine and cysteine and Lysine content were high.

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Monitoring for cephalosporins residues in raw meat in Seoul (서울지역 유통 식육 중의 세팔로스포린계 항균물질 잔류실태 조사)

  • Kim, Mi-Ran;Choi, Yoon-Hwa;Choi, Hoon;Kim, Doo-Hwan;Kim, Young-Seob;Lee, Ju-Hyung
    • Korean Journal of Veterinary Service
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    • v.38 no.4
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    • pp.259-264
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    • 2015
  • We investigated the residues of 6 cephalosporins (cefquinome, cephalexin, cephalonium, cefazolin, ceftiofur, cefuroxime) using LC-MS/MS in raw meat in Seoul. This method involves extraction of the residue from the meat by distilled water and methanol followed by a manual of residue analysis published by the National Institute of Food and Drug Safety Evaluation. The recoveries ranged between 74.71~90.01% in beef, 73.37~101.40% in pork and 70.87~95.53% in chicken, respectively. The limits of detection were 0.0004~0.0563 mg/kg, and the limits of quantification were 0.001~0.169 mg/kg respectively. Residues of cephalosporins which exceeded maximum residue limits (MRL) were not exceed in any of the 287 samples. However, it is necessary to develop multi-method, which includes the active metabolites of ceftiofur.

The Extraction of Manganese from the Medium-Low Carbon Ferromanganese Dust with Nitric Acid (질산에 의한 중.저탄소페로망간제조분진에 함유된 망간의 침출)

  • 이계승;한기천;송영준;신강호;조동성
    • Resources Recycling
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    • v.9 no.1
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    • pp.21-26
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    • 2000
  • Extraction of manganese was investigated with nitric acid from the dust which was generated in the AOD process producing a medium-low carbon ferromanganese from a high carbon ferromanganese. Content of manganese oxide in the dust was about 90%, and phase of it was confirmed as $Mn_3O_4$, The $Mn_3O_4$ particles was agglomerated as spherical shape, and had a lot of pore and crack inside. Maximum recovery of Mn from the sample in the leaching step was about 67% and residue was the amorphous $MnO_2$. The extraction of Mn increased with increasing temperature, but decreased in proportion to concentration of nitric acid. The extraction rate was in good agreement with the pore diffusion model.

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A Study on the Research of Analytical Method for 1,4-Dioxane in Water (1,4-Dioxane의 분석방법 연구)

  • Park, Sun-Ku;Kim, Tae-Ho;Rim, Yeon-taek;Myung, Nho-Il
    • Journal of Korean Society on Water Environment
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    • v.21 no.6
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    • pp.549-563
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    • 2005
  • The study was carried out to develop and standardize the analytical method of 1,4-dioxane in water. The National Institute of Environmental Research in Korea has monitored for 1,4-dioxane in water since 1998 and it has been detected in environmental water occasionally. But the environmental pollution and analytical method in water is not well known over the world. The trace analytical method at low-${\mu}/L$ level is prerequisite in order to evaluate the residue of 1,4-dioxane in water. Evaluation of the method was demonstrated by comparing and analyzing with liquid-liquid extraction, solid-phase extraction and purge & trap technique. As a result of experiment by standard solutions and raw samples, the precision and accuracy for three methods were obtained within error rate of about 10%. Therefore, three methods were standardized as official monitoring method in Korea. Also, a convenient and simple liquid-liquid extraction method for the analysis of 1,4-dioxane in water was developed by combined with gas chromatography/mass spectrometry and applied to the water samples in Korea

A Study on the Remediation of Lead Contaminated Soil in a Clay Shooting Range with Soil Washing (토양세척법에 의한 클레이사격장 납 오염토양의 정화에 관한 연구)

  • Lee, In-Hwa;Seol, Myung-Soo
    • Journal of Soil and Groundwater Environment
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    • v.15 no.5
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    • pp.23-31
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    • 2010
  • For an efficient remediation of Pb-contaminated soil (S-1) in a clay shooting range, a soil washing test was performed with mineral acid, organic acid, chelating agent, and chloride. The Pb extraction efficiency of extractant (0.1 M) used in the washing test showed the order of HCl > $Na_2$-EDTA > NTA > DTPA > citric acid > malic acid > succinic acid > acetic acid > $CaCl_2$ > $MgCl_2$, for S-1 soil. As compared to initial Pb concentration, extraction efficiency by the concentration of extractant was 93.35%, 80.80%, 73.92%, and 24.57% in S-1 soil for HCl (0.5 M, pH 1.10), $Na_2$-EDTA (0.01 M, pH 3.99), citric acid (0.5 M, pH 1.27), and $MgCl_2$ (0.1 M, pH 8.82), respectively. S-1 soil had 56.83% of residue form and 43.17% of non-residue form (18.04% of exchangeable form), respectively. Although the concentrations of these fractions sharply decreased after HCl washing, since the exchangeable forms with relatively large mobility are still distributed as high as 18.78% (to Pb total content in residual soils) in S-1 soil, it is necessary to devise a proper management plan for residual soils after soil washing application.

Optimization of the High-Pressure Condition for Rice Protein Extracting Using Response Surface Methodology (RSM) (반응표면분석법을 이용한 쌀 단백질 초고압 추출조건 최적화)

  • Ra, Ha-Na;Park, Sa-Ra;Kim, Ha-Yun;Cho, Yong-Sik;Kim, Kyung-Mi
    • Journal of the Korean Society of Food Culture
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    • v.34 no.6
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    • pp.779-784
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    • 2019
  • The purpose of this study was to optimize the rice protein extracted using a response surface methodology. The experiment was designed based on a CCD (Central Composite Design), and the independent variables were the high pressure (X1, 0-400 MPa) and processing time (X2, 0-10 minutes). The results of the extraction content (Y1), residue content (Y2), and recovery yield (Y3) were fitted to a response surface methodology model (R2= 0.92, 0.92, and 0.93, respectively). Increasing the pressure and processing time has a positive effect on the extraction content (Y1), residue content (Y2), and recovery yield (Y3). Therefore, these high-pressure conditions (independent variables) can significantly affect the improvement in rice protein extraction efficiency. Thus, the optimal conditions of X1 and X2 were 400 MPa and 10 min., respectively. Under these optimal conditions, the predicted values of Y1, Y2, and Y3 were 62.93, 57.53 mg/g, and 91.76%, respectively.

Development of Multi-residue Analytical Method for 261 Pesticides in Herbal Medicines using GC-MS/MS and LC-MS/MS (GC-MS/MS와 LC-MS/MS를 이용한 생약재 중 261종 농약의 동시분석)

  • Na, Eun Shik;Kim, Seong Soo;Hong, Sung Soo;Kim, Kyoung Ju;Lee, Yong Jae;Lee, Byung Chul;Lee, Kyu Seung
    • Korean Journal of Environmental Agriculture
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    • v.39 no.2
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    • pp.142-169
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    • 2020
  • BACKGROUND: A new analytical method has been developed to determine 261 pesticide residues in herbal medicines. METHODS AND RESULTS: The extraction of pesticides was carried out by modified method of the Korea Food Standards Codex sample extraction and determination was performed using GC-MS/MS and LC-MS/MS. During the pre-treatment process of the test method, Solid-liquid separation was changed to centrifugation. The method was validated by the precision and accuracy results. 261 pesticides spiked at three level 20, 50, 100 ug/kg in herbal medicines. The limit of quantification of method were 4-40 ug/kg for GC-MS/MS and 2-45 ug/kg for LC-MS/MS, respectively. Among the pesticides analysed by GC-MS/MS and LC-MS/MS, 244 pesticides (94% of total number) in chinese matrimony vine and 224 pesticides (86% of total number) in korean angelica root and 231 pesticides (89% of total number) in jujube and 214 (82% of total number) in cnidium showed recoveries in the range of 70-120% with RSD⪯20%. CONCLUSION: These results indicated that GC-MS/MS and LC-MS/MS analysis with the sample extraction in this study can be applied to multi-residue analysis of pesticides in herbal medicines.

Residue Analysis of Quinclorac in Soil by Supercritical Fluid Extraction and Fluorogenic Derivatization Coupled with High Performance Liquid Chromatography (초임계추출과 형광유도체를 이용한 HPLC 에서의 Quinclorac 의 토양중 잔류분석)

  • Kim, Yong-Whan
    • Applied Biological Chemistry
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    • v.40 no.5
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    • pp.442-446
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    • 1997
  • A new analytical method was developed by HPLC after supercritical fluid extraction and fluorogenic derivatization for the determination of quinclorac (3,7-dichloro-8-quinoline carboxylic acid) in soil. The graminicide quinclorac was extracted from soil by supercritical fluid extraction. Supercritical carbon dioxide at 7000 psi $(80^{\circ}C)$ modified with 30% of methanol extracted quinclorac from soil samples at the level of $0.1ng\;g^{-1}$ with 96% recovery. Extracted quinclorac was determined by HPLC as a fluorescent derivative. Derivatization was made with 4-bromomethyl-7-methoxycoumarin (4-Br-Mmc) using 18-crown-6-ether as a catalyst. The conversion was completed within 30 min and the limit of detection was 0.5 ppb to prove that the procedure could be used in the residue analysis of the pesticides containing carboxylic acid group.

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Determination of Ceftiofur Residues by Simple Solid Phase Extraction Coupled with Liquid Chromatography-Tandem Mass Spectrometry in Eel, Flatfish, and Shrimp

  • Kim, Joohye;Shin, Dasom;Kang, Hui-Seung;Lee, Eunhye;Choi, Soo Yeon;Lee, Hee-Seok;Cho, Byung-Hoon;Lee, Kang-Bong;Jeong, Jiyoon
    • Mass Spectrometry Letters
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    • v.10 no.2
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    • pp.43-49
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    • 2019
  • The aim of this study was conducted to develop an analytical method to determine the concentration of ceftiofur residue in eel, flatfish, and shrimp. For derivatization and extraction, the sample was hydrolyzed with dithioerythritol to produce desfuroylceftiofur, which was then derivatized by iodoacetamide to obtain desfuroylceftiofur acetamide. For purification, the process of solid phase extraction (Oasis HLB) was used. The target analytes were confirmed and quantified in $C_{18}$ column using liquid chromatography-tandem mass spectrometry with 0.1% formic acid in water (A) and 0.1% formic acid in acetonitrile (B) as the mobile phase. The linearity of the standard calibration curve was confirmed by a correlation coefficient, $r^2>0.99$. The limit of quantification for ceftiofur was 0.002 mg/kg; the accuracy (expressed as the average recoveries) was 80.6-105%; the precision (expressed as the coefficient of variation) was below 6.3% at 0.015, 0.03, and 0.06 mg/kg. The validated method demonstrated high accuracy and acceptable sensitivity to meet the Codex guideline requirements. The developed method was tested using market samples. As a results, ceftiofur was detected in one sample. Therefore, it can be applied to the analysis of ceftiofur residues in fishery products.