• 제목/요약/키워드: UV spectrometry

검색결과 228건 처리시간 0.024초

UV Spectrometric and DC Polarographic Studies on Apigenin and Luteolin

  • Romanova, Darina;Vachalkiova, Anna
    • Archives of Pharmacal Research
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    • 제22권2호
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    • pp.173-178
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    • 1999
  • Remarks on polyphenolic compounds has been arisen since past few years. the flavonoids appears to be the important groups of compounds with their capability to inhibit DNA damage, lipid peroxidation, to quench free radicals and, at least, anticarcinogenic and antiproliferative effects. On the other hand, their mechanism of action is still unexplained. Apigenin and luteolin are the most wide-spread flavones and they exhibited to be useful in chemoprevention. UV spectrometric and DC polarographic studies on these two compounds have been carried out with regard to changing pH. The most significant changes were observed at basic pH. These results could aid to elucidation of their mechanism of action as pH is one of the important factors for bioprocesses passing in living organisms.

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HPLC/DAD/ESI-MS 및 고체상 추출법을 이용한 뇨시료중 갑상선 호르몬 분석 (Determination of thyroid hormones by solid-phase extraction using high performance liquid chromatograph/diode array detector/electro-spray ionization mass spectrometry in urine samples)

  • 곽선영;문명희;표희수
    • 분석과학
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    • 제19권6호
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    • pp.519-528
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    • 2006
  • 본 연구에서는 뇨시료를 고체상 추출법으로 추출한 후 HPLC/DAD/ESI-MS(high-performance liquid chromatograph/diode array detector/electro-spray ionitation mass spectrometry)를 사용하여 분석하였다. 7종의 thyroid hormones의 HPLC 분리조건은 Hypersil ODS(octadecylsilica) 컬럼(4.6mm I.D., 100 mm length, particle size $5{\mu}m$)을 사용하고 ammonium formate buffer와 acetonitrile을 이동상으로 하여 기울기 용리한 결과 완전 분리가 가능하였으며, UV spectra 및 질량스펙트럼을 확인할 수 있었다. 고체상 추출법에 의한 전처리 최적 조건을 조사한 결과 시료를 pH 3으로 한 후 C18 고체상을 사용하여 4 mL의 methanol/ammonium hydroxide(9:1) 혼합용액으로 용리할 경우 회수율이 89.0-113.1%로 나타났다. HPLC/DAD를 이용하여 10-1000 ng/mL범위에서 검량선을 작성한 결과 $r^2$값은 0.992-0.998 으로 나타났으며 검출한계는 2-4 ng/mL(3.8-13.0 pmol/mL)로 계산되었다.

Direct Analysis in Real Time Mass Spectrometry (DART-MS) Analysis of Skin Metabolome Changes in the Ultraviolet B-Induced Mice

  • Park, Hye Min;Kim, Hye Jin;Jang, Young Pyo;Kim, Sun Yeou
    • Biomolecules & Therapeutics
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    • 제21권6호
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    • pp.470-475
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    • 2013
  • Ultraviolet (UV) radiation is a major environmental factor that leads to acute and chronic reactions in the human skin. UV exposure induces wrinkle formation, DNA damage, and generation of reactive oxygen species (ROS). Most mechanistic studies of skin physiology and pharmacology related with UV-irradiated skin have focused on proteins and their related gene expression or single-targeted small molecules. The present study identified and analyzed the alteration of skin metabolites following UVB irradiation and topical retinyl palmitate (RP, 5%) treatment in hairless mice using direct analysis in real time (DART) time-of-flight mass spectrometry (TOF-MS) with multivariate analysis. Under the negative ion mode, the DART ion source successfully ionized various fatty acids including palmitoleic and linolenic acid. From DART-TOF-MS fingerprints measured in positive mode, the prominent dehydrated ion peak (m/z: 369, M+H-$H_2O$) of cholesterol was characterized in all three groups. In positive mode, the discrimination among three groups was much clearer than that in negative mode by using multivariate analysis of orthogonal partial-least squares-discriminant analysis (OPLS-DA). DART-TOF-MS can ionize various small organic molecules in living tissues and is an efficient alternative analytical tool for acquiring full chemical fingerprints from living tissues without requiring sample preparation. DART-MS measurement of skin tissue with multivariate analysis proved to be a powerful method to discriminate between experimental groups and to find biomarkers for various experiment models in skin dermatological research.

Olefin Metathesis를 이용한 황칠 Essential Oil의 경화 반응에 관한 연구 (Olefin Metathesis Curing Reaction of Essential Oils in Korean Dendropanax Lacquer)

  • 김미리;이원휘;유혜진;김종상;정인우
    • 접착 및 계면
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    • 제16권4호
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    • pp.146-151
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    • 2015
  • 황칠원액을 에탄올로 추출한 황칠의 essential oil을 올레핀 메타테시스(olefin metathesis) 반응의 하나인 ROMP(ring opening metathesis polymerization)법을 이용하여 경화 반응을 수행하였으며, 자연 경화 및 UV 광경화법의 경화 특성 및 경화된 필름의 물성에 대해서 비교 연구하였다. 경화 전후의 황칠의 조성 변화에 대해서 가스 크로마토그래피 질량분석법(GC-MS, gas chromatography mass spectrometry)을 통해 연구하였으며, ROMP법에 의해 경화된 필름의 겔 함량(gel contents, 40%)은 자연 경화(8%)나 UV 광경화법(25%)에 비해 높은 값을 보여주었다. $100^{\circ}C$의 온도 및 2 wt%의 Grubbs' catalyst 조건에서 ROMP 경화반응은 2 h 이내의 경화 반응이 완료되어 자연 경화에 비해 비교적 빠른 경화 속도를 보여주었으며, UV 광경화법에 비해 주름이 없으며 외관상 균일한 도막이 형성됨을 확인하였다. 또한 기존에 경화반응에 참여하는 것으로 알려져 있는 폴리아세틸렌계 성분 이외에 sesquiterpene류인 ${\alpha}$-selinene, ${\beta}$-selinene, ${\delta}$-cadinene 등도 ROMP 경화 반응에 참여함을 확인하였다.

질량분석기 기반-전자코를 이용한 저장중 유채유의 산패 분석 (Rancidity Analysis of Rapeseed Oil under Different Storage Conditions Using Mass Spectrometry-based Electronic Nose)

  • 홍은정;임채란;손희진;최진영;노봉수
    • 한국식품과학회지
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    • 제42권6호
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    • pp.699-704
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    • 2010
  • 유채유에 감광제나 금속이온을 첨가하거나 UV처리를 하였을 때 어떠한 차이가 있는지 알아보기 위하여 MS-전자코를 이용하여 분석하였다. 유채유를 저장하였을 때 저장기간이 증가함에 따라 지방의 품질이 변화되면서 휘발성분이 증감하였는데 판별함수분석(DFA) 결과 DF1값의 영향을 받았으며 품질 변화가 많이 일어날수록 DF1값이 음의 방향으로 이동하였다. 암소에 비하여 UV를 처리하였을 때가 오히려 DF1값의 변화 폭이 크게 나타났다(DF1 $r^2$=0.9481 F=307.07). 실온(17, $26^{\circ}C$)보다는 냉장온도($4^{\circ}C$)에 보관할 때 휘발성분의 변화가 적게 일어났다. 또한 자외선 처리 유무와 온도를 달리 저장할 경우 온도에 의한 영향에 비해 자외선에 의한 영향이 크게 나타났다. ${\gamma}$DF1 값이 암실에서는 각각 $4^{\circ}C$의 경우 0.099, $17^{\circ}C$에서 0.187, $26^{\circ}C$에서 0.278값을 나타냈고 UV 처리 구에서는 각각 $4^{\circ}C$에서 0.554, $17^{\circ}C$는 0.558, $26^{\circ}C$에서는 0.542값을 나타냈다. 감광제인 cytochrome C을 0.1, 0.3, 0.5 mg/%첨가 하였을 때 첨가량이 증가함에 따라 휘발성분의 패턴 변화가 크게 나타났으며 금속이온인 $Cu^{2+}$를 10, 15, 20 mg% 첨가할 경우에도 첨가량이 증가함에 따라 변화가 크게 일어났다. 또한 유채유의 산패 조건에 따른 전자코의 mass spectrum의 감응도 변화는 이미 보고된 GC/MS의 분석 결과와 유사한 pentane, pentanal, 1-pentanol, hexanal, n-octane, 2-hexenal, heptanal, 2-heptenal, decane, 2-octenal, undecane, dodecane과 같은 성분들로 나타났다.

Impurity Profiling and Quantification of Sudan III Dyes by HPLC-selective UV Detection

  • Yang, Ki Ryeol;Hong, Ji Yeon;Yoon, Soo Hwan;Hong, Jongki
    • Bulletin of the Korean Chemical Society
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    • 제35권3호
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    • pp.765-769
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    • 2014
  • An analytical methodology was developed for qualitative and quantitative impurity profiling of the coloring agent Sudan III by high-performance liquid chromatography (HPLC)-diode array detection (DAD). The impurities in commercial Sudan III were characterized by comparison of their retention times and UV spectra with those of authentic standards. Four impurities regulated by International Committees in Sudan III were quantified by HPLC-selective UV detection. The impurities in Sudan dye were successfully separated on a reversed phase C18-column within 25 min and sensitively detected by UV spectrometry at two selective wavelengths. Method validation was conducted to determine linearity, precision, accuracy, and limit of quantification (LOQ). The linear dynamic range extended from 0.002 to 4.0%, with a correlation coefficient (R2) greater than 0.995. The LOQs of the impurities ranged from 8.04 to $54.29{\mu}g/mg$. Based on the established method, the levels of regulated impurities in five commercial Sudan III dyes were determined.

Identification of Loliolide with Anti-Aging Properties from Scenedesmus deserticola JD052

  • Dae-Hyun Cho;Jin-Ho Yun;Jina Heo;In-Kyoung Lee;Yong-Jae Lee;Seunghee Bae;Bong-Sik Yun;Hee-Sik Kim
    • Journal of Microbiology and Biotechnology
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    • 제33권9호
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    • pp.1250-1256
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    • 2023
  • Herein, different extracts of Scenedesmus deserticola JD052, a green microalga, were evaluated in vitro as a potential anti-aging bioagent. Although post-treatment of microalgal culture with either UV irradiation or high light illumination did not lead to a substantial difference in the effectiveness of microalgal extracts as a potential anti-UV agent, the results indicated the presence of a highly potent compound in ethyl acetate extract with more than 20% increase in the cellular viability of normal human dermal fibroblasts (nHDFs) compared with the negative control amended with DMSO. The subsequent fractionation of the ethyl acetate extract led to two bioactive fractions with high anti-UV property; one of the fractions was further separated down to a single compound. While electrospray ionization mass spectrometry (ESI-MS) and nuclear magnetic resonance (NMR) spectroscopy analysis identified this single compound as loliolide, its identification has been rarely reported in microalgae previously, prompting thorough systematic investigations into this novel compound for the nascent microalgal industry.

Qualitative Analysis of the Major Constituents in Traditional Oriental Prescription Bang-poong-tong-sung-san by Liquid Chromatography/Ultraviolet Detector/Ion-Trap Time-of-Flight Mass Spectrometry

  • Eom, Han Young;Kim, Hyung-Seung;Han, Sang Beom
    • Mass Spectrometry Letters
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    • 제5권1호
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    • pp.24-29
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    • 2014
  • An advanced and reliable high performance liquid chromatography (HPLC)/ultraviolet detector (UV)/ion-trap time-of-flight (IT-TOF) mass spectrometry was developed for the simultaneous quantification of 19 marker compounds in Bang-poong-tong-sung-san (BPTS), a traditional oriental prescription. Various parameters affecting HPLC separation and IT-TOF detection were investigated, and optimized conditions were identified. The separation was achieved on a Capcell PAK C18 column ($1.5mm{\times}250mm$, $5{\mu}m$ particle size) using a gradient elution of acetonitrile and water containing 0.1% formic acid at a flow rate of 0.1 mL/min. The column temperature was maintained at $40^{\circ}C$ and the injection volume was $2{\mu}L$. IT-TOF system was equipped with an electrospray ion source (ESI) operating in positive or negative ion mode. The optimized electrospray ionization parameters were as follows: ion spray voltage, +4.5 kV (positive ion mode), or -3.5 kV (negative ion mode); drying gas ($N_2$), 1.5 L/min; heat block temperature, $200^{\circ}C$. Automatic $MS^n$ (n = 1~3) analyses were carried out to obtain structural information of analytes. Elemental compositions and their mass errors were calculated based on their accurate masses obtained from a formula predictor software. The marker compounds in BPTS were identified by comparisons between $MS^n$ spectra from standards and those from extracts. Moreover, the libraries of $MS^2$ and $MS^3$ spectra and accurate masses of parent and fragment ions for marker compounds were constructed. The developed method was successfully applied to the BPTS extracts and identified 17 out of 19 marker compounds in the BPTS extracts.

LC-Tandem Mass Spectrometry를 활용한 농업용수 중 Perfluorochemicals 분석시료 전처리법 (Sample Preparation Method for Perfluorochemicals with LC-Tandem Mass Spectrometry in Agricultural Water)

  • 김진효;진초롱;최근형;박병준
    • 농약과학회지
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    • 제19권1호
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    • pp.1-4
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    • 2015
  • 잔류성 유기오염물질인 과불화합물 중 perfluorooctanesufonic acid (PFOS)와 perfluorooctanoic acid (PFOA)의 잔류분석은 환경부 "잔류성 유기오염물질 공정시험기준"에 따라 hydrophilic-lipophilic balance (HLB) solid phase extraction (SPE) 전처리 후 LC-$MS^n$를 이용해 정량 분석하고 있다. 본 연구에서는 환경부 설정 공정시험법에 따라 농업용수 전처리 후, 시험법에서 제거하지 못한 미지의 불순물을 Envi-Carb$^{TM}$을 통해 회수율에 영향을 주지 않고 손쉽게 제거하였다. 또한, 과불화합물 분석에 사용되는 LC-$MS^n$ 중 quadrupole-time-of-flight mass spectrometry (qTOFMS)에서 측정된 PFCs의 정량한계를 평가한 결과, 시험에 사용된 장비간 정량한계 편차가 크게 관찰되었으나, 시험대상 장비 모두 농업용수 중 ng/L 수준으로 잔류하는 과불화합물의 정밀 잔류분석에 사용가능 한 것으로 확인되었다.

토양 및 고체시료 중 불소함량 측정기법 (A Review on the Analytical Techniques for the Determination of Fluorine Contents in Soil and Solid Phase Samples)

  • 안진성;김주애;윤혜온
    • 한국지하수토양환경학회지:지하수토양환경
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    • 제18권1호
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    • pp.112-122
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    • 2013
  • Current status of soil contamination with fluorine and its source were investigated. The basic principles and procedures of various techniques for the analysis of fluorine contents in soil and solid phase samples were summarized in this review. Analysis of fluorine in solid matrices can be achieved by two types of techniques: (i) UV/Vis spectrophotometer or ion selective electrode (ISE) analysis after performing appropriate extraction steps and (ii) direct solid analysis. As the former cases, the standard method of Korean ministry of environment, alkali fusion-ISE method, pyrohydrolysis, oxygen bomb combustion, aqua regia digestion-automatic analysis, and sequential extraction-ISE method were introduced. In addition, direct analysis methods (i.e., X-ray fluorescence spectrometry and proton induced gamma-ray emission spectrometry) and atomic spectrometry combining with the equipment for introducing solid phase sample were also reviewed. Fluorine analysis techniques can be reasonably selected through site-specific information such as matrix condition, contamination level, the amount of samples and the principles of various methods for the analysis of fluorine presented in this review.