• 제목/요약/키워드: Reversed phase chromatography

검색결과 347건 처리시간 0.025초

PVC 포장재에서 식품유사용매와 식품으로 이행되는 알킬페놀 (Migration of Alkylphenols from PVC Food Packaging Materials to Food Simulants and Foods)

  • 이선희;임흥열;신효선
    • 한국식품과학회지
    • /
    • 제33권4호
    • /
    • pp.416-422
    • /
    • 2001
  • 식품포장용 PVC제인 wrap, sheet 및 gasket으로부터 식품 유사용매와 식품으로 이행되는 알킬페놀류를 HPLC와 GC/MSD로 분석하였다. 세 가지 모든 재질에서 7개의 nonyl phenol 이성질체만이 검출되었고 다른 알킬페놀류는 검출되지 않았으며, wrap이 sheet와 gasket보다 그 함량이 높았다. 각 포장재질로부터 수용성 식품유사용매(증류수, 4% acetic acid, 20% ethanol)와 지용성 식품유사용매(n-heptane)에 의한 nonyl phenol의 용출량은 처리온도 $60^{\circ}C$보다는 $95^{\circ}C$에서, 수용성보다는 지용성 식품유사용매에서 각각 많았고, 또한 wrap에서 sheet와 gasket보다 그 양이 많았다. PVC gasket을 사용한 과일쥬스, olefin계 gasket을 사용한 유아용 쥬스, olefin계 병마개를 사용한 음료에서 nonyl phenol이 각각 포장재로부터 이행되었으며, 포장하기 전의 이들 식품에서도 nonyl phenol이 검출되었다.

  • PDF

Bacillus subtilis AH18의 고추역병 방제능과 $Siderophore_{AH18}$의 구조분석 (Structural Identification of $Siderophore_{AH18}$ from Bacillus subtilis AH18, a Biocontrol agent of Phytophthora Blight Disease in Red-pepper)

  • 우상민;김상달
    • 한국미생물·생명공학회지
    • /
    • 제36권4호
    • /
    • pp.326-335
    • /
    • 2008
  • Bacillus subtilis AH18균주는 auxin, siderophore 그리고 cellulase를 동시에 생산하는 PGPR 균주이자 생물방제균주로 항진균성 siderophore의 특성을 확인한 결과 catechol type의 siderophore로 확인하였다. $Siderophore_{AH18}$ 의 정제는 Amberlite XAD-2, sephadex LH-20 column chromatography 그리고 HPLC를 통해 정제 및 정제여부를 확인하였으며, GC-MS, $^1H$-NMR, 그리고 $^{13}C$-NMR을 통해 구조 및 분자량을 확인하였다. 그 결과 B. subtilis AH18이 생산하는 siderophore은 분자량 883의 bacillibactin임을 확인하였으며, 포자발아억제활성을 나타냄을 확인하였다. B. subtilis AH18은 P. capsici에 의한 고추역병을 효과적으로 방제하였으며(방제력 55%), 이는 bacillibactin에 의한 효과가 포함되리라 추측된다.

Simultaneous Determination of Polycyclic Aromatic Hydrocarbons and Their Nitro-derivatives in Airborne Particulates by Using Two-dimensional High-performance Liquid Chromatography with On-line Reduction and Fluorescence Detection

  • Boongla, Yaowatat;Orakij, Walaiporn;Nagaoka, Yuuki;Tang, Ning;Hayakawa, Kazuichi;Toriba, Akira
    • Asian Journal of Atmospheric Environment
    • /
    • 제11권4호
    • /
    • pp.283-299
    • /
    • 2017
  • An analytical method using high-performance liquid chromatography (HPLC) with fluorescence (FL) detection was developed for simultaneously analyzing 10 polycyclic aromatic hydrocarbons (PAHs) and 18 nitro-derivatives of PAHs (NPAHs). The two-dimensional HPLC system consists of an on-line clean-up and reduction for NPAHs in the 1st dimension, and separation of the PAHs and the reduced NPAHs and their FL detection in the 2nd dimension after column-switching. To identify an ideal clean-up column for removing sample matrix that may interfere with detection of the analytes, the characteristics of 8 reversed-phase columns were evaluated. The nitrophenylethyl (NPE)-bonded silica column was selected because of its shorter elution band and larger retention factors of the analytes due to strong dipole-dipole interactions. The amino-substituted PAHs (reduced NPAHs), PAHs and deuterated internal standards were separated on polymeric octadecyl-bonded silica (ODS) columns and by dual-channel detection within 120 min including clean-up and reduction steps. The limits of detection were 0.1-9.2 pg per injection for PAHs and 0.1-140 pg per injection for NPAHs. For validation, the method was applied to analyze crude extracts of fine particulate matter ($PM_{2.5}$) samples and achieved good analytical precision and accuracy. Moreover, the standard reference material (SRM1649b, urban dust) was analyzed by this method and the observed concentrations of PAHs and NPAHs were similar to those in previous reports. Thus, the method developed here-in has the potential to become a standard HPLC-based method, especially for NPAHs.

Quantitative Analytical Method for Eighteen Marker Compounds in Ongyeong-tang, a Traditional Herbal Formula, Using High-Performance Liquid Chromatography for Quality Assessment

  • Kim, Jung-Hoon;Shin, Hyeun-Kyoo;Seo, Chang-Seob
    • 대한본초학회지
    • /
    • 제30권4호
    • /
    • pp.11-20
    • /
    • 2015
  • Objectives : Ongyeong-tang (OGT) is a traditional herbal formula used to cure gynaecological disorders. OGT consists of 12 herbal medicines containing various bioactive components. Therefore, the development of suitable analytical method for the marker compounds is necessary for the quality control of OGT. Methods : Determination of the 18 marker compounds in OGT preparations was quantitatively performed by high-performance liquid chromatography-photodiode array detection analysis. The marker compounds were separated on a reversed-phase C 18 column and the analytical method was successfully validated, which was applied to compare OGT extracts from laboratory preparation and commercial OGT granules. Results : Limit of detection and limit of quantification values were in the ranges of $0.001-0.016{\mu}g/mL$ and $0.003-0.047{\mu}g/mL$, respectively. Precision was 0.03-3.71 % within a day and 0.03-3.81 % over four consecutive days. Recovery of marker compounds ranged from 90.63-108.26 %, with relative standard deviation (RSD) values < 4.0 %. Reproducibility was < 2.5 % of the RSD value. The 18 marker compounds were stable within 16 h at $10^{\circ}C$, with the RSD value < 3.5 %. Quantitative analysis results showed that the quantities of the 18 marker compounds varied among OGT samples. Pearson coefficient evaluation and principal component analysis demonstrated that an OGT water extract produced by a laboratory method clearly differed from commercial OGT granules. Conclusions : The developed analytical method was simple, precise, and reliable. Therefore, it can be used for the quality assessment of OGT preparations.

Quantitative Determination of Compounds from Akebia quinata by High-Performance Liquid Chromatography

  • Yen, Nguyen Thi;Thu, Nguyen Van;Zhao, Bing Tian;Lee, Jae Hyun;Kim, Jeong Ah;Son, Jong Keun;Choi, Jae Sui;Woo, Eun Rhan;Woo, Mi Hee;Min, Byung Sun
    • Bulletin of the Korean Chemical Society
    • /
    • 제35권7호
    • /
    • pp.1956-1964
    • /
    • 2014
  • To provide the scientific corroboration of the traditional uses of Akebia quinata (Thunb.) Decne., a detailed analytical examination of A. quinata stems was carried out using a reversed-phase high performance liquid chromatography (RP-HPLC) method coupled to photodiode array detector (PDA) for the simultaneous determination of four phenolic substances; cuneataside D (1), 2-(3,4-dihydroxyphenyl)ethyl-O-${\beta}$-D-glucopyranoside (2), 3-caffeoylquinic acid (3) and calceolarioside B (4). Particular attention was focused on the main compound, 3-caffeoylquinic acid (3), which has a range of biological functions. In addition, 2-(3,4-dihydroxyphenyl)ethyl-O-${\beta}$-D-glucopyranoside (2) was considered as a discernible marker of A. quinata from its easy confuse plants. The contents of compounds 2 and 3 ranged from 0.72 to 2.68 mg/g and from 1.66 to 5.64 mg/g, respectively. The validation data indicated that this HPLC/PDA assay was used successfully to quantify the four phenolic compounds in A. quinata from different locations using relatively simple conditions and procedures. The pattern-recognition analysis data from 53 samples classified them into two groups, allowing discrimination between A. quinata and comparable herbs. The results suggest that the established HPLC/PDA method is suitable for quantitation and pattern-recognition analyses for a quality evaluation of this medicinal herb.

Radical Scavenging Activity and Content of Cynarin (1,3-dicaffeoylquinic acid) in Artichoke (Cynara scolymus L.)

  • Jun, Neung-Jae;Jang, Ki-Chang;Kim, Seong-Cheol;Moon, Doo-Young;Seong, Ki-Cheol;Kang, Kyung-Hee;Tandang, Leoncia;Kim, Phil-Hoon;Cho, So-Mi K.;Park, Ki-Hun
    • Journal of Applied Biological Chemistry
    • /
    • 제50권4호
    • /
    • pp.244-248
    • /
    • 2007
  • The contents of total phenol and total flavonoid of artichoke (Cynara scolymus L.) were measured. The antioxidant activity of the artichoke was evaluated based on its potential as a scavenging the ABTS radical. These results showed the antioxidant activity of artichoke has a close relationship with the total flavonoid content. The compound showing antioxidant activity was isolated from the artichoke by repeated column chromatography and recrystallization. Based on the spectrometric studies, the compound was identified as 1,3-dicaffeoylquinic acid, known as cynarin. The content of cynarin from heads and leafs of the artichoke determined by $C_{18}$ reversed phase HPLC (high-performance liquid chromatography) coupled with photodiode array detector was 10.15 and 0.67 mg/g, respectively. This compound showed potent antioxidant activities against DPPH and ABTS radicals ($EC_{50}$ = 14.09 and 28.85 ${\mu}M$, respectively).

A Comprehensive Identification of Synaptic Vesicle Proteins in Rat Brains by cRPLC/MS-MS and 2DE/MALDI-TOF-MS

  • Lee, Won-Kyu;Kim, Hye-Jung;Min, Hye-Ki;Kang, Un-Beom;Lee, Cheol-Ju;Lee, Sang-Won;Kim, Ick-Young;Lee, Seung-Taek;Kwon, Oh-Seung;Yu, Yeon-Gyu
    • Bulletin of the Korean Chemical Society
    • /
    • 제28권9호
    • /
    • pp.1499-1509
    • /
    • 2007
  • Proteomic analyses of synaptic vesicle fraction from rat brain have been performed for the better understanding of vesicle regulation and signal transmission. Two different approaches were applied to identify proteins in synaptic vesicle fraction. First, the isolated synaptic vesicle proteins were treated with trypsin, and the resulting peptides were analyzed using a high-pressure capillary reversed phase liquid chromatography/tandem mass spectrometry (cRPLC/MS/MS). Alternatively, proteins were separated by two-dimensional gel electrophoresis (2DE) and identified by matrix-assisted laser desorption ionization mass spectrometry (MALDI-TOF/MS). Total 18 and 52 proteins were identified from cRPLC/MS-MS and 2DE-MALDI-TOF-MS analysis, respectively. Among them only 2 proteins were identified by both methods. Of the proteins identified, 70% were soluble proteins and 30% were membrane proteins. They were categorized by their functions in vesicle trafficking and biogenesis, energy metabolism, signal transduction, transport and unknown functions. Among them, 27 proteins were not previously reported as synaptic proteins. The cellular functions of unknown proteins were estimated from the analysis of domain structure, expression profile and predicted interaction partners.

Simultaneous Determination of Amitraz, Bromopropylate, Coumaphos, Cymiazole and 2,4-Dimethylaniline in Korean Honey Samples by High-Performance Liquid Chromatography

  • Ryoo, Jae-Jeong;Kim, Se-Hoon;Jeong, Young-Han;Do, Hwan-Suk;Ryu, Jeong-Eun;Kwon, Hae-Young;Jeong, Ji-Yoon;Park, Hye-Jin;Lee, Soon-Ho;Hong, Moo-Ki;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
    • /
    • 제29권5호
    • /
    • pp.1043-1047
    • /
    • 2008
  • Simultaneous determination of amitraz, bromopropylate, coumaphos, cymiazole and 2,4-dimethylaniline in 200 honey samples purchased in Korea was performed by reversed-phase high-performance liquid chromatography with multiple UV detection. 2% Acetone in hexane was used for a liquid-liquid extraction and 20-40% water in acetonitrile solutions were used as mobile phases. The LOD for the analytes varied between 0.4 and 1.5 $\mu$g/L and the recoveries were yielded between 64 and 94%. Relative standard deviation of the repeatability of the method is less than 15%. Amitraz was not present in amount above 10 $\mu$ g/L and one for coumaphos and cymiazole and two for bromopropylate, and three for 2,4-dimethylanilne were detected in amount above 10 $\mu$ g/ L. Levels of the acaricide residues found were less than 50 $\mu$ g/L.

Sphingosine Kinase Assay System with Fluorescent Detection in High Performance Liquid Chromatography

  • Jin, You-Xun;Yoo, Hwan-Soo;Kihara, Akio;Choi, Chang-Hwan;Oh, Seik-Wan;Moon, Dong-Cheul;Igarashi, Yasuyuki;Lee, Yong-Moon
    • Archives of Pharmacal Research
    • /
    • 제29권11호
    • /
    • pp.1049-1054
    • /
    • 2006
  • Activation of Sphingosine kinase (Sphk) increases a bioactive lipid, sphingosine 1-phosphate (S1P) and has been observed in a variety of cancer cells. Therefore, inhibition of Sphk activity was an important target for the development of anticancer drugs. As a searching tool for Sphk inhibitor, we developed fluorescent Sphk activity assay combined with high performance liquid chromatography (HPLC). Previously we established murine teraticarcinoma mutant F9-12 cells which lack S1P lyase and stably express Sphk1. By using F9-12 cells, optimal assay conditions were established as follows; $100\;{\mu}M\;of\;C_{17}-Sph\;and\;30\;{\mu}g$ protein of F9-12 cells lysate in 20 min. Sphingosine analog $C_{17}-Sph$ was efficiently phosphorylated by Sphk activity ($K_{m}:67.08\;{\mu}M,\;V_{max}\;:1507.5\;pmol/min/mg$). New product $C_{17}-S1P$ was separated from S1P in reversed-phase HPLC. In optimized conditions, 300 nM of phorbol 12-myristate 13-acetate (PMA) increased Sphk activity approximately twice while $20\;{\mu}M$ of N,N-dimethylsphingosine (DMS) reduced 70% of Sphk activity in F9-12 cells lysate. In conclusion, we established non-radioactive but convenient Sphk assay system by using HPLC and F9-12 cells.

고성능 액체 크로마토그래피를 이용한 고삼 중의 oxymatrine 분석에 관한 연구 (Determination of oxymatrine in Sophora Radix by High Performance Liquid Chromatography)

  • 양승권;윤영자;남궁미옥
    • 분석과학
    • /
    • 제17권4호
    • /
    • pp.289-294
    • /
    • 2004
  • 고성능 액체 크로마토그래피를 이용하여 고삼 중의 oxymatrine을 분석하였다. acetonitrile을 포함하는 완충용액과 $C_{18}$컬럼을 이용한 역상 크로마토그래피를 수행하였다. Oxymatrine의 분리는 215 nm에서 UV흡수가 관측되었다. 고삼 중의 oxymatrine의 추출은 다양한 용매와 다양한 추출방법을 사용한 결과, 마쇄한 고삼의 최적의 추출 효율은 $80^{\circ}C$에서 50% ethanol로 5시간 동안 환류가열 하였을 때 가장 높은 효율을 보였다. 대부분의 추출 방법은 복잡한 전처리를 필요로 하지만, 본 연구에서는 승화 추출법으로 복잡한 전처리를 제외시킨 추출법을 고안하였다. 승화 추출은 높은 진공 ($1{\times}10^{-3}$ torr) 과 높은 온도 ($200^{\circ}C$)에서 수행되었다. 승화 추출법을 사용한 추출 효율은 다른 추출 방법들과 비교해서 전처리 과정을 거치지 않은 장점은 있었으나 추출 효율이 좀 낮았다.