• Title/Summary/Keyword: Sep-pak $C_{18}$

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Optimization of Automated Solid Phase Extraction-based Synthesis of [18F]Fluorocholine (고체상 추출법을 기반으로 한 [18F]Fluorocholine 합성법의 최적화 연구)

  • Jun Young PARK;Jeongmin SON;Won Jun KANG
    • Korean Journal of Clinical Laboratory Science
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    • v.55 no.4
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    • pp.261-268
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    • 2023
  • [18F]Fluorocholine is a radiopharmaceutical used non-invasively in positron emission tomography to diagnose parathyroid adenoma, prostate cancer, and hepatocellular carcinoma by evaluating the choline metabolism. In this study, a radiolabeling method for [18F]fluorocholine was optimized using a solid phase extraction (SPE) cartridge. [18F]Fluorocholine was labeled in two steps using an automated synthesizer. In the first step, dibromomethane was reacted with [18F]KF/K2.2.2/K2CO3 to obtain the intermediate [18F]fluorobromomethane. In the second step, [18F]fluorobromomethane was passed through a Sep-Pak Silica SPE cartridge to remove the impurities and then reacted with N,N-dimethylaminoethanol (DMAE) in a Sep-Pak C18 SPE cartridge to label [18F]fluorocholine. The reaction conditions of [18F]fluorocholine were optimized. The synthesis yield was confirmed according to the number of silica cartridges and DMAE concentration. No statistically significant difference in the synthesis yield of [18F]fluorocholine was observed when using four or three silica cartridges (P>0.05). The labeling yield was 11.5±0.5% (N=4) when DMAE was used as its original solution. On the other hand, when diluted to 10% with dimethyl sulfoxide, the radiochemical yield increased significantly to 30.1±5.2% (N=20). In conclusion, [18F]Fluorocholine for clinical use can be synthesized stably in high yield by applying an optimized synthesis method.

Determination of Aldehydes in Tap Water by Reverse Phase Liquid Chromatography (역상 액체 크로마토그래피에 의한 수도수 중 알데하이드류의 정량)

  • Choi, Yong Wook;Choi, Yun Jung
    • Journal of the Korean Chemical Society
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    • v.43 no.4
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    • pp.438-446
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    • 1999
  • The optimum analytical method of aldehydes, ozone by-products, was established by reverse phase liquid chromatography. Six aldehydes including formaldehyde, acetaldehyde, acrolein, propionaldehyde, butylaldehyde and benzaldehyde, and one ketone including acetone were selected as aldehyde test samples through preliminary experiments. Such analytical conditions as the pH of citrate buffer solution, reaction temperature, reaction time, and concentration of DNPH, the component and composition of desorption solvent were optimized. As the result, pH 3.0 of citrate buffer solution, 40$^{\circ}C$ of reaction temperature, 15 minutes of reaction time, and 0.012% of DNPH concentration were chosen as optimum conditions. Aldehydes-DNPH derivatives in water were concentrated on $C_18$ Sep-Pak cartridge and followed by elution of their derivatives fraction with THF/ACN(70/30) mixture, and showed recoveries of the range from 87 to 107%. Separation condition on Nova-Pak $C_18$ column with low pressure gradient elution from ACN/MeOH/water(30/10/60) of an initial condition to 80% ACN of a final condition was found to give a good resolution within 20 minutes of run time. 86% to 103% of recovery for aldehydes using this method was similar to that for aldehyde using EPA Method 554 which is ranged from 84% to 103%.

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Optimization of HPLC Method and Clean-up Process for Simultaneous and Systematic Analysis of Synthetic Color Additives in Foods (식품 중 타르색소의 동시분석 및 계통분석을 위한 HPLC 분석조건 및 정제과정 확립)

  • Park, Sung-Kwan;Hong, Yeun;Jung, Yong-Hyun;Lee, Chang-Hee;Yoon, Hae-Jung;Kim, So-Hee;Lee, Jong-Ok
    • Korean Journal of Food Science and Technology
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    • v.33 no.1
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    • pp.33-39
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    • 2001
  • To develop a method for separation process using Sep-pak $C_18$, simultaneous and systematic analysis of 8 permitted and 11 non-permitted synthetic food colors in Korea, optimization of analysis conditions for reverse phase ion-pair high performance liquid chromatography was carried out. For the best result of Sep-pak $C_18$ separation the pH of color standard mixture solution was $5{\sim}6$ and 0.1% HCl-methanol solution were set as eluent. The colors eluated from Sep-pak $C_18$ cartridge were determined and confirmed by high performance liquid chromatography with a photodiode array detector at 420 nm for yellow colors type, at 520 nm for red colors type, at 600 nm for blue and green colors type and at 254 nm for mixed colors. Conditions for HPLC analysis were as follows: column, Symmetry $C_18$ (5 m, 3.9 mm $i.d.{\times}150\;mm$); mobile phase, 0.025 M ammonium acetate (containing 0.01 M tetrabutylammonium bromide) : acetonitrile : methanol (65 : 25 : 10) and 0.025 M ammonium acetate(containing 0.01 M tetrabutylammonium bromide) : acetonitrile : methanol (40 : 50 : 10); flow rate, 1 mL/min. It takes 35 minutes for simultaneaus analysis and 18 minutes for systematic analysis. The detection limits range of each colors were $0.01{\sim}0.05\;{\mu}g/g$.

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Simultaneous Analytical Techniques for Determination of 8 Synthetic Food Colors in Foods by HPLC (HPLC를 이용한 식품중 식용타르색소 8종의 동시분석)

  • Park, Sung-Kwan;Lee, Chang-Hee;Park, Jae-Seok;Yoon, Hae-Jung;Kim, So-Hee;Hong, Yeun;Lee, Jong-Ok;Lee, Chul-Won
    • Analytical Science and Technology
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    • v.13 no.3
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    • pp.378-384
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    • 2000
  • This Study has been carried out to develop a method of analysis of 8 permitted synthetic food colors [including Brilliant Blue FCF(B1), Indigocarmine (B2), Fast green FCF(G3), Amaranth (R2), Erythrosine (R3), Allura red (R40), Tartrazine (Y4), Sunset Yellow FCF (Y5)] in Korean foods by HPLC. After adjusting to 0.5% HCl, each of the food colors extracted was eluted by Sep-pak $C_{18}$ cartridge. Eluates were then determined by high performance liquid chromatograph with a UV-VIS detector. Recoveries of the 8 synthetic food colors were found to be 81.2-98.0% for soft drinks, 80.6-96.1% for candy, 79.8-96.3% for chewing gum, 76.5-91.7% for cereals, 79.9-93.8% for ice cream and 78.6-94.7% for jelly, respectively. The detection limits were $0.05-0.1{\mu}g/g$.

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UV-HPLC Determination of Carbowyl Group Using 2-Bromoacetyltriphenylene as a Pre-labeling Reagent - The isolative determination of prostaglandin $E_2$ and $F_2{\alpha}$ by HPLC (2-Bromoacetyltriphenylene 유도체화제를 이용한 카르복실기 함유성분의 분석법 (I) - 프로스타글란딘 $E_2$$F_2{\alpha}$ 혼합물의 HPLC에 의한 분리정량)

  • 이왕규;정해수;김박광
    • YAKHAK HOEJI
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    • v.30 no.6
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    • pp.311-316
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    • 1986
  • A new UV labeling reagent was developed and used in HPLC for the determination of prostaglandin $E_2$ which have weak UV light-absorbing property. This reagent, 2-bromoacetyltriphenylene, was synthesized by the bromination of 2-acetyltriphenylene which was obtained from triphenylene by Friedel-Crafts reaction. The wave length maximum (${\lambda}_{max}^{CH_3CN}$ of this reagent was 268nm. Prostaglandin E$_2$ was extracted from prostaglandin E$_2$-$\beta$-cyclodextrin using a Sep-pak $C_{18}$ cartridge. The prostaglandin E$_2$ was labeled with 2-bromoacetyl-triphenylene in aectonitrite using 18-crown-6-ether as catalyst. Derivatized prostaglandins were separated on a reversed-phase column (Radial-pak) $\mu$-Bondapak $C_{18}$ using acetonitrile: water=60:40 as mobile phase. The effluent was monitored by UV detector at 254nm filter kit. Linearity of calibration curve was obtained between 30ng and 140ng, and the lower limit of detection was 5ng.

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Isolation of a starfish myorelaxant peptide (SMP) isotype from the pyloric caeca of Patiria pectinifera

  • Kubarova, Anastasia;Go, Hye-Jin;Park, Nam Gyu
    • Fisheries and Aquatic Sciences
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    • v.24 no.4
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    • pp.163-170
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    • 2021
  • Peptides are naturally occurring biological molecules that are found in all living organisms. These biologically active peptides play a key role in various biological processes. The aim of this study is the extraction and the purification of bioactive materials that induce relaxation of an apical muscle from the pyloric caeca of Patiria pectinifera. The acidified pyloric caeca extract was partially separated by the solid phase extraction using a stepwise gradient on Sep-Pak C18 cartridge. Among the fractions, materials eluted with 60% methanol/0.1% trifluoroacetic acid was put a thorough of a series of high performance liquid chromatography (HPLC) steps to isolate a neuropeptide with relaxation activity. The purified compound was eluted at 28% acetonitrile in 0.1% trifluoroacetic acid with retention time of 25.8 min on the CAPCELL-PAK C18 reversed-phase column. To determine the molecular weight and the amino acid sequence of the purified peptide, LC-MS and Edman degradation method were used, respectively. The primary structure of the peptide was determined to be FGMGGAYDPLSAGFTD which corresponded to the amino acid sequence of a starfish myorelaxant peptide (SMP) isotype (SMPb) found in the cDNA sequence encoding SMPa and its isotypes. In this study, a muscle relaxant neuropeptide (SMPb) has been isolated from pyloric caeca of starfish P. pectinifera. This is the first report of SMPb isolation on the protein level from P. pectinifera.

Antioxidant Properties of Polyphenol Fractions from Cranberry Powder in LPS-Stimulated RAW264.7 Cells (LPS로 자극한 RAW264.7 세포에서 크랜베리 폴리페놀 분획물의 항산화 효과)

  • Jung, Hana;Lee, Kiuk;Hwang, Keum Taek;Kwak, Ho-Kyung
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.8
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    • pp.1241-1247
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    • 2015
  • The objective of this study was to determine antioxidant properties of polyphenol fractions of cranberry powder employing lipopolysaccharides (LPS)-stimulated RAW264.7 macrophage cells. Ethyl acetate fraction (EF) and methanol fraction (MF) of cranberry powder were prepared using a C18 Sep-Pak cartridge. When cells were treated with LPS for 20 h, intracellular reactive oxygen species (ROS) and DNA damage significantly increased. In cells pre-treated with EF, MF, and total fraction (TF: combining EF and MF), significant reductions of intracellular ROS were observed. The tested fractions reduced LPS-induced DNA damage measured by Hoechst staining. In addition, LPS-induced DNA oxidation was attenuated when cells were pre-treated with TF and MF. However, there was no significant difference in LPS-induced superoxide dismutase activity.

Quantitative Analysis of trans-Resveratrol in Red Wines by Solid Phase Extraction and LC/MS (고체상 추출법과 LC/MS를 이용한 적포도주 중의 trans-Resveratrol 분석)

  • Park, Gyo-Beom;Moon, Hyoung-Sil;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.16 no.2
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    • pp.125-133
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    • 2003
  • In order to determine the contents of trans-resveratrol in red wine, which was mainly consumed in Korea, both LC/MS-ESI and LC/MS-APCI methods were used after solid-phase (Sep-Pak $C_{18}$-cartridges) extraction. The contents of trans-resveratrol obtained by LC/MS-ESI were detected in the range of $0.06-4.31{\mu}g/mL$. The recoveries were ranged from 88.4 to 97.9%. The values of relative standard deviation were ranged from 0.6 to 4.6% and the detection limit was $0.001{\mu}g/mL$. The contents of trans-resveratrol obtained by LC/MS-APCI were detected in the range of $0.09-4.02{\mu}g/mL$ and the detection limit was $0.005{\mu}g/mL$.

Separation and Determination of Acteoside in Pedicularis resupinata var. oppositifolia by Ion Pair Liquid Chromatography (이온쌍 액체 크로마토그래피에 의한 마주송이풀 중의 Acteoside의 분리와 정량)

  • Yun, Young Ja;Yu, Gu Yong
    • Analytical Science and Technology
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    • v.8 no.2
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    • pp.161-166
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    • 1995
  • Determination of acteoside in Pedicularis resupinata var. oppositifolia has been studied using ion pair liquid chromatography. Sample was extracted with 40mL methanol for 4 hrs. The extract was cleaned up by using Sep-Pak $C_{18}$ catridge and 8mL aqueous methanol eluent(methanol 50%, water 50%, phosphate buffer pH=8.0). Its determination was performed by means of IP-HPLC with a Hamilton PRP-1 polystyrene-divinylbenzene reversed phase column($15cm{\times}4.6mm$ i. d., $5{\mu}m$) and an aqueous methanol eluent(methanol 60%, water 40% phosphate buffer pH=8.2) containing of $5.0{\times}10^{-3}M$ tetrabutylammonium bromide. The established method was applied to the sample that was collected in area of Pyung Chang gun. As a result, its content ranges showed to be 0.062~0.076%.

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Study on the Antimicrobial Substances of Lactic Acid Bacteria Isolated from Pig's intestine (돼지의 장에서 불리한 유산균의 항시균 활성물질에 관한 연구)

  • Seo, Jeong-Yong;Chung, Myung-Hee;Kim, Young-Jun
    • Journal of the Korea Organic Resources Recycling Association
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    • v.17 no.4
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    • pp.59-65
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    • 2009
  • The antimicrobial activity-possessing materials were screened in the cell free supernatant (CFS) of fourteen lactic acid-fermenting strains isolated from pig's intestine. Each cell free supernatant of cultured strains was treated with various proteinases, heat, and/or alkali (NaOH). The antimicrobial activities were remained even after the enzyme and heat treatment but disappeared after neutralization with 1M NaOH, implying that the materials would be organic acids rather than proteins. Further purification of CFS through solid phase extraction using Sep-pak $C_{18}$ Cartridges and high performance anion exchange chromatography using Bio-LC system revealed that four organic acids, such as oxalic acid, citric acid, lactic acid, and acetic acid, were the main materials for the activity. Lactic acid was the highest amount in all organic acids, ranging from 54% to 77%. This strongly implies that the lactic acid would be the primary material for the antimicrobial activity in all tested strains.

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