• Title/Summary/Keyword: extraction chromatography

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Evaluation of Tar Dyes Used in Commercial Foods (식품 중 합성첨가물 사용실태 조사 연구 -타르색소 중심으로-)

  • 윤미혜;김국주;김정임;황선일;문수경;정은주;김재관
    • Journal of Food Hygiene and Safety
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    • v.15 no.2
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    • pp.108-113
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    • 2000
  • This study was carried out to propose a simple method for the extraction of seven tar dyes such as tartrazine, sunset yellow FCF, amaranth, erythrosine, allura red, brilliant blue FCF and indigo carmine using aminopropyl amine cartridge and to determine the content of the dyes in candies, soft drinks, ice bars and okchuns produced in Korea. The tar dyes were simultaneously analyzed by reverse phase high performance liquid chromatography(HPLC). The recovery rates of the dyes ranged from 65.8% to 99.6%. The contents of the dyes in candies, soft drinks, ice bars and octhuns were N.D.∼50.1 mg/kg, N.D.∼49.9 mg/kg, N.D.∼56.0 mg/kg and N.D.∼867.3 mg/kg, respectively. The types of the dyes used most frequently for candies, soft drinks and ice bars were tartrazine, brilliant blue and amaranth, respectively. Of the samples, tartrazine was used frequently, and indigo carmine was not used at all.

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Glycomacropeptide Hydrolysed from Bovine K-Casein ; II. Chromatographic Changes of k-Casein Macropetide as Related to Trichloroacetic Acid Concentration (우유의 k-Casein에서 분해된 Glycomacropeptide에 관한 연구; II. Trichloroacetic Acid의 농도에 따른 k-Casein Macropeptide 분별 특성의 변화)

  • Moon Yong-Il;Lee Wonjae;Oh Sejong
    • Food Science of Animal Resources
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    • v.25 no.4
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    • pp.478-482
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    • 2005
  • Bovine k-casein macropeptide was prepared by adding TCA (3, 6, and $12\%$) treatment after chymosin reaction. Each TCA soluble macropeptide was fractionated into five peak by ion exchange column chromatography. In proportiion to TCA concentrations, the ratio of peak area showed different the elution pattern. At the 6 and $12\%$ TCA concentration, area ratio of P-I which did not content carbohydrates was decreased to 19.9 and $17.0\%$ of total peak area respectively. The area of P-III was changed from $10.2\%\;to\;26.2\;and\;13.2\%$ when the TCA concentration was increased from 3 to 6 and $12\%$ Cholera toxin binding activity of k-casein macropeptide eluted at $0.17\~0.18M$ NaCl gradient was not inhibited by 6 and $12\%$ TCA treatments. The use of $6\%$ TCA as extraction buffer was feasible and led to an effective separation of the peak III.

Changes of Volatile Components in Alaska Pollack Sik-hae during Low-Temperature Fermentation (전통 명태식해 저온숙성 중 휘발성 성분의 변화)

  • Cha, Yong-Jun;Jeong, Eun-Jeong;Kim, Hun;Lee, Young-Mi;Cho, Woo-Jin
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.31 no.4
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    • pp.566-571
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    • 2002
  • Volatile flavor compounds in Alaska pollack sik-hae during fermentation at 5$^{\circ}C$ were analyzed by liquid-liquid continuous extraction (LLCE) and gas chromatography/mass spectrometry (GC/MS) methods. Sixty five volatile compounds were detected in Alaska pollack sik-hae during fermentation. These compounds were composed mainly of 11 S-containing compounds, 13 alcohols, 13 acids, 4 aldehydes, 4 ketones, 6 terpenes,4 aromatic compounds and 10 miscellaneous compounds. Among these, 9 S-containing compounds (3-(methylthio)-1-propene, dimethyl disulfide, diallyl sulfide, methylallyl disulfide, methyl-(E) -propenyl disulfide, dimethyl trisulfide, 2 diallyl disulfide isomers and diallyl trisulfide), 2 acids (acetic acid and butanoic acid), 2 ketones (2, 3-butanedione and 6-methyl-5-hepten-2-one) and 2 esters (ethyl formate and ethyl acetate) were significantly increased during fermentation (p<0.05), and these compounds were suspected to affect on the odor of Alaska pollack sik-hae.

Effect of γ-Irradiation on the Volatile Organic Compounds from Leek (Allium tuberosum R.) (부추(Allium tuberosum R.)의 감마선 조사에 의한 휘발성 유기화합물의 성분 변화)

  • Han, Byung-Jae;Yang, Sook-Young;Kim, Jun-Hyoung;Shim, Sung-Lye;Gyawali Rajendra;Lee, Sung-Jin;Kim, Kyong-Su
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.34 no.4
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    • pp.513-518
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    • 2005
  • Volatile compounds of $\gamma-irradiation$ leeks (Aillum tuberosum R.) were isolated by simultaneous steam distillation and extraction method (SDE) and analyzed by gas chromatography/mass spectrometry (GC/MS) along with the non-irradiated sample. Leeks were irradiated at dose of 20 kGy and non-irradiated samples were considered as control sample. 56 and 54 compounds were identified in non-irradiated and irradiated samples, respectively. These components included the functional groups; alcohols, aldehydes, esters, ketones, N- and S-containing compounds. S-containing compounds such as dimethyl trisulfide, methyl-(Z)-l-proenyl trisulfide, dimethyl disulfide, 3-ethyl-l,2-dithi-5-ene and methyl allyl disulfide were the major compounds. Methyl-(Z)-l-propenyl trisulfide, diallyl trisulfide, (E)-2-hexanal and 3-ethyl-l,2-dithi-5-ene were clearly decreased by the $\gamma-irradiation$, but dimethyl disulfide, diallyl sulfide, allyl methyl sulfide and pyridine were increased by the $\gamma-irradiation$.

Analysis of 1,4-Dioxane and Chlorohydrins in Food Additives by Purge & Trap GC (퍼지앤트랩-기체크로마토그래피(PT-GC)를 이용한 식품첨가물 중 1,4-디옥산 및 클로로히드린류 분석)

  • 조태용;신영민;반경녀;오세동;이창희;이영자;문병우
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.32 no.7
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    • pp.965-970
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    • 2003
  • This study has been performed to develope a method for the simultaneous determination of 1,4-dioxane (DOX), epichlorohydrin (EPC), propylene chlorohydrin (PCH), ethylene chlorohydrin (ECH) and 1,3-dichloro-2-pro-panol (DCP) in polysorbates, chloline chloride, choline bitartrate, modified starch and spices by purge and trapgas chromatography. Experimental design was used to select a suitable trap by measuring the limit of detection (LOD) and to investigate the effect of temperature and salt of extraction, and the percentage of recovery in various matrix. The LOD of DOX, EPC, PCH, ECH and DCP were 1.38$\mu\textrm{g}$, 0.23$\mu\textrm{g}$, 3.30$\mu\textrm{g}$, 3.97$\mu\textrm{g}$, 20.43$\mu\textrm{g}$ respectively, by means of using Vorcarb 3000 trap with 5$0^{\circ}C$ sample sparger. Excluding EPC, the recoveries of target compounds were above 90% in all matrix. Target compounds in polysorbates (17), choline chloride (5), choline bitartrate (5), modified starch (8) and spices (25) were not detected. But 2.5 ppm of DOX was detected in Tween 80.

Immune-Enhancing Effects of Polysaccharides Isolated from Ascidian (Halocynthia roretzi) Tunic (우렁쉥이(Halocynthia roretzi) 껍질로부터 분리된 다당류의 면역증강 효과)

  • Lee Dae-Hoon;Hong, Joo-Heon
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.5
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    • pp.673-680
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    • 2015
  • In this study, the immune-enhancing effects of purified polysaccharides from ascidian (Halocynthia roretzi) tunic were investigated. Crude polysaccharides (AP) were isolated by enzyme extraction (neutrase, $60^{\circ}C$, 15h), ethanol precipitation, and lyophilization. In addition, crude polysaccharides were further fractionated into unabsorbed fractions (APF-I, fraction No. 11~17) and absorbed fractions (APF-II, fraction No. 22~37) by DEAE-sepharose CL-6B column chromatography in order to isolate immune regulating polysaccharide. The major constituents in APF-I and APF-II were total sugar (66.62% and 27.03%), uronic acid (47.53% and 15.87%), hexosamine (16.62% and 46.79%), and protein (2.43% and 4.94%), respectively. APF-I increased production of nitric oxide (NO) and cytokines, such as tumor necrosis factor-alpha (TNF-${\alpha}$) and interleukin (IL)-6 in a dose-dependent manner. The mRNA expression levels of inducible NO synthetase, cyclooxygenase-2, TNF-${\alpha}$, and IL-6 were markedly increased as determined by polymerase chain reaction analysis. The above data led us to conclude that macrophage activation of purified polysaccharides was higher than that of crude polysaccharides. The polysaccharides isolated from ascidian tunic investigated herein are useful as natural immune enhancing agents.

Application of Freezing Filtration Method to the Analysis of Alkylphenols, Chlorophenols and Bisphenol a in Korean Aquatic Biological Samples Using GC/MS-SIM (GC/MS-SIM을 이용한 우리나라 수중 생물시료 중 알킬페놀, 클로로페놀과 비스페놀 A의 분석을 위한 냉동필터법의 응용)

  • Kim, Hyub;Jang, Cheol-Hyeon
    • Journal of Korean Society of Environmental Engineers
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    • v.29 no.6
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    • pp.689-698
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    • 2007
  • A new technique was proposed for the determination of alkylphenols, chlorophenols and bisphenol A in korean aquatic biological samples. The alkylphenols, chlorophenols and bisphenol A in korean aquatic biological samples were extracted with acetonitrile and then acetonitrile layer was refrigerated at $-60^{\circ}C$ for 2 hours(freezing filtration method). Also, solid-phase extraction(SPE) was used to XAD-4 and subsequent conversion to isobutoxycarbonyl(isoBOC) or tert-butyldimethylsilyl(TBDMS) derivatives for sensitive analysis with gas chromatography/mass spectrometry-selected ion monitoring(GC/MS-SIM) mode. For isoBOC derivatization and TBDMS derivatization the recoveries were $70.1\sim150.6%$ and $93.8\sim108.3%$, the method detection limit(MDLs) of bisphenol A for SIM were $0.062{\mu}g/kg$ and $0.010{\mu}g/kg$, and the SIM respectively. When these methods were applied to korean aquatic biological samples, the concentrations of the 11 phenolic EDCs were $0.675\sim1.970{\mu}g/kg$.

Persistent Organic Pollutants (POPs) Residues in Greenhouse Soil and Strawberry Organochlorine Pesticides (딸기 시설재배지 토양 및 농산물 중 잔류성유기오염물질(POPs)의 잔류량 - 유기염소계 농약)

  • Lim, Sung-Jin;Oh, Young-Tak;Jo, You-Sung;Ro, Jin-Ho;Choi, Geun-Hyoung;Yang, Ji-Yeon;Park, Byung-Jun
    • Korean Journal of Environmental Agriculture
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    • v.35 no.1
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    • pp.6-14
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    • 2016
  • BACKGROUND: Residual organochlorine pesticides (OCPs) are chemical substances that persist in the environment, bioaccumulate through the food web, and pose a risk of causing adverse effect to human health and the environment. They were designated as persistent organic pollutants (POPs) by Stockholm Convention. Greenhouse strawberry is economic crop in agriculture, and its cultivation area and yield has been increased. Therefore, we tried to investigate the POPs residue in greenhouse soil and strawberry.METHODS AND RESULTS: Extraction and clean-up method for the quantitative analysis of OCPs was developed and validated by gas chromatography (GC) with electron capture detector (ECD). The clean-up method was established using the modified quick, easy, cheap, effective, rugged, and safe(QuEChERS) method for OCPs in soil and strawberry. Limit of quantitation (LOQ) and recovery rates of OCPs in greenhouse soil and strawberry were 0.9-6.0 and 0.6-0.9 μg/kg, 74.4-115.6 and 75.6-88.4%, respectively. The precision was reliable sincerelative standard deviation (RSD) percentage (0.5-3.7 and 2.9-5.2%) was below 20, which was the normal percent value. The residue of OCPs in greenhouse soil was analyzed by the developed method, and dieldrin, β-endosulfan and endosulfan sulfate were detected at 1.6-23, 2.2-28.4 and 1.8-118.6 μg/kg, respectively. Those in strawberry were not detected in all samples.CONCLUSION: Dieldrin, β-endosulfan and endosulfan sulfate in a part of investigated greenhouse soil were detected. But those were not detected in investigated greenhouse strawberry. These results showed that the residue in greenhouse soil were lower level than bioaccumulation occurring.

Muscle tissue Distribution Level of Ampicillin in Olive flounder(Paralichthys olivaceus), Rockfish(Sebastes schlegeli), and Red sea bream(Pagrus major) following oral administration (Ampicillin의 경구투여에 따른 양식 어류(넙치, 조피볼락, 참돔)의 근육조직내 잔류량의 변화)

  • Cho Yoon-Hee;Jung Won-Chul;Shin Yong-Woon;Kim Kyoung-Won;Ha Ji-Young;Heo Sung-Hyek;Kim Eui-Gyung;Chung Hee-Sik;Kang Seok-Joong;Choi Yu-Jeong;Kim Suk;Lee Hu-Jang
    • Journal of Veterinary Clinics
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    • v.23 no.2
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    • pp.164-168
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    • 2006
  • The residue depletion of ampicillin was investigated in the olive flounder (Paralichthys olivaceus), rockfish (Sebastes schlegeli), and red sea bream (Pagrus major) after 5 days treatment with medicated feed at a dose of 100 mg/kg bw/day. Fishes were sampled for muscle on 1st, 2nd, 3rd, and 4th day after treatment. Ampicillin concentrations were determined by high performance liquid chromatography after SPE column extraction. The recovery rates of ampicillin in muscle samples ranged 94-98% and 83-88% for the concentration of 0.05 mg/kg and 0.1 mg/kg, respectively. Ampicillin concentrations detected on 1st day after treatment were 0.143, 0.138, and 0.187 mg/kg in the muscle of olive flounder, rockfish, and red sea bream, respectively. After a withdrawal of 3 days, muscle concentrations were 0.016, 0.012, and 0.021 mg/kg in the olive flounder, rockfish, and red sea bream, respectively. Ampicillin was not detectable in muscle samples on 4 days following withdrawal of the medicated feed. From results of the present study, a withdrawal period of ampicillin is proposed on 5 days after 5 days treatment with medicated feed at a dose of 100 mg/kg bw/day to avoid the presence of excessive residues of the edible muscles of olive flounder, rockfish, and red sea bream.

Estimation of Measurement Uncertainty for the HPLC Analysis of Deoxynivalenol in Wheat (밀에서 HPLC에 의한 데옥시니발레놀 분석의 측정불확도 산정)

  • Ok, Hyun-Ee;Chang, Hyun-Joo;Ahn, Jang-Hyuk;Cho, Jae-Young;Chun, Hyang-Sook
    • Korean Journal of Food Science and Technology
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    • v.41 no.3
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    • pp.258-264
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    • 2009
  • The principal objective of this study was to estimate the measurement uncertainty associated with determination of deoxynivalenol (DON), a mycotoxin generated by Fusarium strain, in food. In service of this goal, wheat as a food matrix was analyzed via high performance liquid chromatography-ultraviolet (HPLC-UV) detection using an immunoaffinity column for clean-up. The uncertainty sources in the measurement process were identified by sample weight, final volume, and sample concentration in extraction volume with components including standard stock solution, working standard solution, 5 standard solutions, calibration curve, matrix, and instrument. The expanded uncertainty for DON at a concentration of 300 ${\mu}g/kg$ was estimated as 71.62 ${\mu}g/kg$ using a coverage factor of two, which provides a confidence level of approximately 95%. The most influential component in the uncertainty sources was the recovery of the wheat matrix, followed by the calibration curve. These results indicate that all efforts may be directed toward reducing the uncertainties of the recovery of the wheat matrix and the calibration curve to obtain a reliable HPLC-UV method for DON analysis in wheat.