• 제목/요약/키워드: extraction chromatography

검색결과 1,300건 처리시간 0.032초

Analysis of tetracyclines in shrimp samples based on a two-step extraction approach prior to high-performance liquid chromatography

  • Thinnakorn Sukkhunthod;Thanakorn Pluangklang;Sumita Boonnab;Sira Sansuk;Phitchan Sricharoen;Maliwan Subsadsana
    • 분석과학
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    • 제37권4호
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    • pp.211-219
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    • 2024
  • This study presents a sensitive and reliable method for determining tetracycline (TC), oxytetracycline (OTC), and chlortetracycline (CTC) residues in shrimp samples. A two-step process involving liquid-liquid extraction (LLE) followed by solid-phase extraction (SPE) was developed prior to HPLC analysis. The target analytes were effectively extracted using EDTA/McIlvaine buffer (pH 4.0): methanol (80:20, %v/v), with subsequent clean-up using a C18 SPE cartridge. HPLC separation was conducted on a C18 column (250 mm × 4.6 mm i.d., 5 ㎛) at 30 ℃, using 0.01 % trifluoroacetic acid (A) and acetonitrile (B) as the mobile phase. A gradient elution protocol was applied, transitioning from 85(A):15(B) %v/v to 70(A):30(B) %v/v at 7 min, with a 5 min hold, followed by adjustment to 85(A):15(B) %v/v for 13-14 min. The detection was performed using photodiode array (PDA) at 365 nm with a flow rate of 1.0 mL/min. The calibration curves exhibited good linearity within a concentration range of 0.4-6.0 ㎍/mL (R2 > 0.995). The limits of detection (LOD) for TC, OTC, and CTC in shrimp were 0.034, 0.029, and 0.021 ㎍/mL, respectively. The limits of quantitation (LOQ) for TC, OTC, and CTC were found to be 0.114, 0.097, and 0.071 ㎍/mL, respectively. Recoveries of TC, OTC, and CTC from spiked shrimp samples ranged from 91.0 % to 95.5 %, 92.4 % to 97.2 %, and 93.3 % to 96.6 %, respectively. This method was successfully applied to the determination of TC, OTC, and CTC residues in shrimp samples sourced from various local markets.

Bacillus sp. YJ-63이 생산하는 항곰팡이성 항생물질의 단리

  • 신영준;정명주;정영기
    • 한국생물공학회:학술대회논문집
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    • 한국생물공학회 2000년도 춘계학술발표대회
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    • pp.509-511
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    • 2000
  • An antifungal antibiotic was produced from Bacillus sp. YJ-63, and antibiotic was purified to a homogeneity by butanol extraction, Silica-gel column chromatography, Sephadex LH-20 gel filtration column chromatography and HPLC. The purified antibiotic showed one spot on Thin Layer Chromatography, which was negative to ninhydrin and positive to iodine. This finding indicated that the antibiotic was a cyclopeptide structure. UV absorption spectrum of the antibiotic in methanol was maximal at 277 nm, which corresponded to the spectrum for all of the Iturin antibiotic. The antibiotic was stable up to $121^{cdot}C$ and in the range of pH $3.O{\sim}l2.0$ with a stable of ${\alpha}-amino$ acid and ${beta}-amino$ acid, and showed high activity for fungi and yeasts,

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Streptomyces sp. KIS13 균주에서 분리한 thiol계 단백질분해효소 저해물질의 특성 (Characterization of Thiol Protease Inhibitor Isolated from Streptornyces sp. KISl3)

  • 김인섭;이계준
    • 한국미생물·생명공학회지
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    • 제18권5호
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    • pp.501-505
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    • 1990
  • 토양으로부터 분리한 Streptomyces 속 세균 KIS 13은 thiol 계통 단백질분해효소 활성을 특이적으로 저해하는 저분저량 저해물질을 생성하였다. 저해물질 생성은 세균체성장에 연관된 생성양상이 나타내었다. 배양액으로부토 butanol 추출, silicagel 60 column chromatography, Sephadex LH-2 gel-filtration chromatography, preparative HPLC 등의 과정을 통하여 단백질 분해효소 저해물질을 순수분리하였다. 이 저해물질은 Hammersten casein을 기질로 사용할때, papain에 대하여 non-competitive한 저해양상을 나타내었다.

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Analysis of flavonoids in the mature fruit of Vaccinium uliginosum L. of China

  • Hua, Lian Li;Yoshitama, Kunijiro
    • Advances in Traditional Medicine
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    • 제6권1호
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    • pp.65-67
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    • 2006
  • In this study, a new extraction method was developed and two kinds of flavonoids were extracted from the mature fruit of Vaccinium uliginosum L. of China. These two kinds of flavonoids were analyzed by spectral and identified by high-performance liquid chromatography (HPLC) and UV/Vis. The extract of the fruit was total acid hydrolyzed. TLC chromatography was subsequently employed to identify the hydrolysate. Two kinds of aglycone flavonoids, quercetin and myricetin, were identified. At the same time PC chromatography was used to identify the monomer sugar in the flavonoids and it was verified as glucose. HPLC, UV/Vis, and Mass spectrum analyses revealed that the flavonoids were quercetin 3-monoglucosides and myricetin 3-monoglucosides.

방선균 분리주 G-37이 생산하는 항생물질의 물리.화학적 특성과 항균활성 (Physico-chemical and Antagonistic Properties of Antibiotics Produced by Actinomycetes Isolate G-37)

  • 여운형;김영호;채순용;박은경
    • 한국연초학회지
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    • 제17권2호
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    • pp.103-108
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    • 1995
  • Antibiotic and physico-chemical properties of an active compound from actinomycetes isolate G-37, of which the culture filtrate had an inhibitory effect against tobacco mosaic virus(W) infection, were examined. The active compound, which was purified by ethylacetate extraction, silica gel column chromatography, preparative thin layer chromatography, and high performance liquid chromatography, showed strong antibacterial activities especially against Gram-positive bacteria including Bacillus subtillis, Sarcina lutea and Staphylococcus aureus. From the IH-NMR, FAB/RfS, UV spectral data, and physicochemical properties, the active compound of G-37 appears to belong to a peptide antibiotic group. Among the known peptide antibiotics in the antibiotic group, No. 280, A-30912, and Taitomycin showed molecular weights and ultra violet spectrum similar to those of the active compound from G-37, but was not identical to the compound, which suggests that it may be a new peptide antibiotics.

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한우 초유로부터 Lactoferrin의 분리.정제 (Isolation and Purification of Lactoferrin from Korean Native Cow's Colostrum)

  • 양희진;하월규;양동훈;박기문;이수원
    • 한국축산식품학회지
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    • 제20권2호
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    • pp.125-132
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    • 2000
  • Lactoferrin was isolated from the colostrum of Korean native cow by using several purification steps such as batch extraction, ion exchange chromatography, gel filtration chromatography and affinity chromatography. Other whey protein components that having similar molecular weight and affinity to lactoferrin were gradually removed from crude Korean native cow's lactoferrin during the purification steps. The amount of lactoferrin collected from a liter of Korean native cow's colostrum was 65mg and the recovery rate was 29.4%. The molecular weight of the purified Korean native cow's lactoferrin was estimated approximately 81,000dalton.

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Isolation of Fucosterol from Pelvetia siliquosa by High-speed Countercurrent Chromatography

  • Hwang, Seung Hwan;Jang, Jai Man;Lim, Soon Sung
    • Fisheries and Aquatic Sciences
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    • 제15권3호
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    • pp.191-195
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    • 2012
  • We report here the use of high-speed countercurrent chromatography (HSCCC) in the preparative isolation and purification of the bioactive component, fucosterol, from Pelvetia siliquosa. A crude extract was obtained by ultrasonic extraction of powdered P. siliquosa using methylene chloride and was then subjected to separation and purification by HSCCC, coupled with evaporative light-scattering detection. Preparative HSCCC was performed successfully using a two-phase solvent system, n-heptane:methanol (3:2, v/v), to obtain 10.96 mg fucosterol with 96.8% purity from 50 mg of crude extract; the recovery rate was approximately 90.5%.

생리활성물질 S-627(A)와 S-627(B)의 분리 (Isolation of S-627(A) and (B) as Candidates of Anticandiosis Agent)

  • 이상한;이동선;서영배;김종국;홍순덕
    • 생명과학회지
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    • 제7권3호
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    • pp.186-191
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    • 1997
  • 수정된 선별법(modified selection method)을 사용하여 candiosis에 대한 새로운 생리활성물질(anticandiosis agent)을 생성하는 미생물을 분리하여Streptomyces sp. S627이라 명명하였으며, 이균의 발효액으로부터 methanol추출, diaion Hp-20, silica gel chromatography, 및 분취용 TLC 등의 방법을 사용하여 물리화학적 특성이 다른 S-637(A)와 S-627(B)을 분리하였다.

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Optimization of Extraction Conditions and Quantitative Analysis of Isoquercitrin and Caffeic Acid from Aster scaber

  • Lee, Ju Sung;Quilantang, Norman G.;Nam, Kung-Woo;Piao, Xiang-Lan;Chung, Mi Ja;Lee, Sanghyun
    • Natural Product Sciences
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    • 제24권3호
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    • pp.199-205
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    • 2018
  • To determine the optimum extraction conditions that give the highest yield of isoquercitrin and caffeic acid from Aster scaber, the effects of four extraction variables (solvent concentrations, extraction time, number of repeated extraction, and solvent volumes) on isoquercitrin and caffeic acid yield was examined via HPLC-UV. Our results showed that the highest extract and isoquercitrin yield were observed when A. scaber was extracted with 450 mL distilled water for 8 hr repeatedly for three times. In case of caffeic acid, the content was higher in the two repeated extracts. Also, content analysis of isoquercitrin in Aster species was performed in which A. fastigiatus, A. ageratoides, and A. scaber exhibited the highest isoquercitrin content at 6.39, 5.68, and 2.79 mg/g extract, respectively. In case of caffeic acid, the highest content of A. scaber and A. glehni was 0.64 and 0.56 mg/g extract, respectively. This study reports an optimized method for extraction of isoquercitrin and caffeic acid from A. scaber and evaluates potential sources of the compounds.

Characterization of the Yellow Croaker Larimichthys polyactis muscle Oil Extracted with Supercritical Carbon Dioxide and an Organic Solvent

  • Lee, Joo-Hee;Asaduzzaman, A.K.M.;Yun, Jun-Ho;Yun, Jun-Hyun;Chun, Byung-Soo
    • Fisheries and Aquatic Sciences
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    • 제15권4호
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    • pp.275-281
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    • 2012
  • Yellow croaker Larimichthys polyactis muscle oil was extracted using an environmental friendly solvent, supercritical carbon dioxide (SC-$CO_2$), in a semi-batch flow extraction process. SC-$CO_2$ was applied at temperature $35^{\circ}C$ to $45^{\circ}C$ and $150^{\circ}C$ to $250^{\circ}C$ bar of pressure. The flow rate of $CO_2$ (27.79 g/min) was constant throughout the entire 1.5 h extraction period. The oil extraction yield was influenced by the physical properties of SC-$CO_2$ at different temperatures and pressures. The extracted oil was analyzed by gas chromatography to determine the fatty acid composition. According to our results, the SC-$CO_2$ extracted oil was high in eicosapentaenoic acid and docosahexaenoic acid. In addition, the SC-$CO_2$ extracted oil showed greater stability than n-hexane extracted oil based on the peroxide value and acid value. Thus, the quality of yellow croaker oil obtained by SC-$CO_2$ extraction was slightly higher than that of oil obtained by n-hexane extraction.