• 제목/요약/키워드: UV detection

검색결과 551건 처리시간 0.035초

카르복시펩티다제A의 에스테르 가수분해 반응생성물의 종류에 대한 외부 및 분자내 친핵체의 영향. 아실-효소중간체의 포획시도 (Effect of External and Intramolecular Nucleophiles on Nature of Products of Carboxypeptidase A-Catalyzed Hydrolysis of Esters. Attempted Trapping of Acyl-Enzyme Intermediate)

  • 서정헌
    • 대한화학회지
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    • 제22권3호
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    • pp.164-172
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    • 1978
  • 상온에서 카르복시펩티다제 A에 의한 에스테르 기질의 가수분해 반응을 여러가지 외부 시약의 존재하에 행하였다. 산무수물 형태의 아실-효소중간체가 외부시약에 의해 공격받는다면 아실 부분에 포획된 생성물이나 효소부분에 포획된 생성물이 형성될 것이다. 반응생성물의 분광도와 효소활성도의 변화를 조사한 결과 포획반응의 생성물은 검출되지 않았다. 또한, O-(o-hydroxyphenylacetyl)-L-${\beta}$-phenyllactate가수분해에 대한 효소 반응속도변수를 측정하였다. 이 기질의 o-히드록시기가 분자내 포획기로서 작용하여 산무수물형태의 아실-효소중간체를 공격하여 20coumaranone이 형성되었나를 조사하였으나 분자내 포획반응이 일어났다는 증거는 얻지 못하였다. 이러한 중간체 포획반응의 실패는 포획용 시약이 아실-효소 중간체의 무수산기에 접근할때 입체적 방해를 받거나 중간체의 가수분해 단계도 효소에 의해 촉매되기 때문이라고 생각된다.

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Emission Plasma Spectroscopy of High-pressure Microdischarges

  • 이병준;주영도;김승환;하태균;공형섭;박용정;박종도;남상훈
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2014년도 제46회 동계 정기학술대회 초록집
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    • pp.253.2-253.2
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    • 2014
  • Micro hollow cathode discharges (MHCDs) are high-pressure, non-equilibrium discharges. Those MHCDs are useful to produce an excimer radiation. A major advantage of excimer sources is their high internal efficiency which may reach values up to 40% when operated under optimum conditions. To produce strong excimer radiation, the optimisation of the discharge conditions however needs a detailed knowledge of the properties of the discharge plasma itself. The electron density and temperature influence the excitation as well as plasma chemistry reactions and the gas temperature plays a major role as a significant energy loss process limiting efficiency of excimer radiation. Most of the recent spectroscopic investigations are focusing on the ultraviolet or vacuum ultraviolet range for direct detection of the excimer. In our experiments we have concentrated on investigating the micro hollow cathodes from the near UV to the near infrared (300~850 nm) to measure the basic plasma parameters using standard plasma diagnostic techniques such as stark broadening for electron density and the relative line intensity method for electron temperature. Finally, the neutral gas temperature was measured by means of the vibrational rotational structures of the second positive system of nitrogen.

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GC/MS를 이용한 수질환경시료 중 personal care products의 분석 (Determination of personal care products in aquatic environmental samples by GC/MS)

  • 이인정;이철구;허성남;이재관
    • 분석과학
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    • 제23권5호
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    • pp.477-484
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    • 2010
  • 항균제 및 자외선 차단물질, 유기인계 난연제 등과 같은 personal care products는 개인이 일상생활에서 광범위하게 사용하는 비누, 화장품, 치약 등에 포함된 합성유기화합물로 하 폐수 처리시설에서 완벽하게 제거되지 않고 생활하수에 포함된 상당수의 양이 환경 중으로 배출되고 있다. 외국사례의 경우 하천, 해양, 토양, 저질, 생물상 등 다양한 환경매체에서 검출되고 있으며, 잔류성 생물농축성이 있어 지속적으로 노출시 생태계 및 인간의 건강에 심각한 영향을 끼칠 우려가 있다. 본 연구에서는 수질환경시료 중 15종의 personal care products를 액-액추출하여 GC/MS로 분석하였으며, 방법검출한계는 $0.004\sim0.273\;{\mu}g/L$의 범위를 나타내었다. 하천수에서는 TCEP, TCPP 등 2종이 검출되었으며, 하수처리장 시료에서는 triclosan, 4-MBC, EHMC, BP-3, TCEP, TPP, TBEP 등 7종이 검출되었다.

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.

2005년 6월의 서울시 대기의 포름알데히드 농도분포 특징 (Distributions of Formaldehyde in Seoul in June, 2005)

  • 황정훈;이미혜;이강웅;한진석
    • 한국대기환경학회지
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    • 제22권1호
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    • pp.63-71
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    • 2006
  • An automated carbonyl measurement system was constructed. Atmospheric carbonyl compounds were extracted onto DNPH containing collection solution while flowing through a glass coil. Each carbonyl species was separated on a HPLC column and quantified by UV absorption detector. Using this system, carbonyl compounds were continuously measured at the campus of Korea University in Seoul, Korea during June, 2005. Sampling resolution was 30 minutes and the detection limit of HCHO was 0.19 ppbv. Also, $\O_{3}$, it's precursors, and meteorological parameters were measured. The maximum, minimum, average, and median concentrations of HCHO during the whole experiment was 35.8 ppbv, 1.4 ppbv, 11.7 ppbv, and 9.3 ppbv respectively. Formaldehyde showed a distinct diurnal variation with a broad maximum around 13 $\sim$ 15, which was 1 $\sim$ 3 hours ahead of an ozone maximum. During a couple of days, however, HCHO concentrations were kept high through the night or increased concomitantly with NOx in the morning. These results imply that HCHO was mainly produced from the photochemical oxidation of VOCs, but local emission sources couldn't be ruled out. The differences between daily maximum and minimum of $O_{3}$ and HCHO were calculated for 11 days of June, when typical diurnal variations were observed for the two species. A strong positive correlation was found between $\Delta O_{3}$ and $\Delta HCHO$ and the average mole ratio of $\Delta HCHO$ to $\Delta O_{3}$ was 2.6. It indicates that formaldehyde played a key role in $\Delta O_{3}$ production as an indicator species in Metropolitan Seoul during June, 2005.

Determination of nadolol enantiomers in human plasma using a coupled achiral-chiral high-performance liquid chromatography method

  • Lee, Seung-Beom;Pham, Thuy-Vy;Mai, Xuan-Lan;Le, Thi-Anh-Tuyet;Nguyen, Thi-Ngoc-Van;Kang, Jong-Seong;Mar, Woongchon;Kim, Kyeong Ho
    • 분석과학
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    • 제33권2호
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    • pp.59-67
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    • 2020
  • Nadolol is a β-blocker drug, which effectively manages hypertension and angina pectoris. Its chemical structure allows the formation of four possible stereoisomers. A coupled column high-performance liquid chromatographic (HPLC) system with UV and fluorescence detection was investigated for simultaneously determining four nadolol enantiomers in human plasma. The plasma samples were prepared using a convenient liquid-liquid extraction process and passed through HPLC. Nadolol was initially separated from the endogenous compounds or other impurities in human plasma on a Phenomenex silica column, and its enantiomers were resolved and determined on a Chirapak AD-H column. The developed HPLC method achieved an effective chiral separation and significantly eliminated endogenous compound interference. This optimal HPLC method was validated following FDA guidelines. The results showed good selectivity, linearity, accuracy (90.50 % - 105.27 %), and precision (RSDs < 9.52 %) for each enantiomer. This method was also successfully applied to determine nadolol enantiomers in the plasma samples of a healthy male volunteer (after orally administering 80 mg racemic nadolol), proving its suitability for nadolol stereoselective pharmacokinetic studies.

느타리버섯, 양송이버섯, 팽이버섯 추출물의 핵산 관련 물질 함량 분석 (Contents of Nucleic Acids(Nucleosides and Mono-Nucleotides) in Extracts of Pleurotus ostreatus, Agaricus bisporus and Flammulina velutipes)

  • 김명숙;김건희
    • 한국식품영양학회지
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    • 제23권3호
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    • pp.376-380
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    • 2010
  • 본 연구는 버섯에 정미 성분 및 기능성 성분으로 작용하는 핵산 관련 성분의 분석을 위하여 느타리, 양송이, 팽이버섯을 동결 건조한 뒤 열수 추출 및 효소적 가수분해과정을 거친뒤 HPLC로 정성 및 정량하였다. 연구 결과, 8종류의 핵산 관련 성분의 정성 및 정량 분석을 위한 효과적인 분석 조건을 확립하였으며, 버섯에 함유되어 있는 핵산 관련 성분은 cytidine, uridine, inosine, guanosine, 5'-UMP, 5'-GMP 및 5'-IMP 7종으로 분석되었다. 각각의 핵산 관련 성분 함량 분석 결과는 양송이 ($26.06{\pm}0.01\;mg/g$)>느타리($24.13{\pm}1.01\;mg/g$)>팽이버섯($18.84{\pm}0.03\;mg/g$)의 순으로 나타났으며, 그 중 cytidine 및 inosine 성분이 가장 많이 함유되어 있는 것으로 나타났다.

Synthesis and Characterization of Novel pH-Sensitive Hydrogels Containing Ibuprofen Pen dents for Colon-Specific Drug Delivery

  • Mahkam, Mehrdad;Poorgholy, Nahid;Vakhshouri, Laleh
    • Macromolecular Research
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    • 제17권9호
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    • pp.709-713
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    • 2009
  • The aim of this study was to develop novel intestinal specific drug delivery systems with pH sensitive swelling and drug release properties. The carboxyl group of ibuprofen was converted to a vinyl ester group by reacting ibuprofen and vinyl acetate as an acylating agent in the presence of catalyst. The glucose-6-acrylate-1, 2, 3, 4-tetraacetate (GATA) monomer was prepared under mild conditions. Cubane-1, 4-dicarboxylic acid (CDA) linked to two 2-hydroxyethyl methacrylate (HEMA) group was used as the crosslinking agent (CA). Methacrylic-type polymeric prodrugs were synthesized by the free radical copolymerization of methacrylic acid, vinyl ester derivative of ibuprofen (VIP) and GATA in the presence of cubane cross linking agent. The structure of VIP was characterized and confirmed by FTIR, $^1H$ NMR and $^{13}C$ NMR spectroscopy. The composition of the cross-linked three-dimensional polymers was determined by FTIR spectroscopy. The hydrolysis of drug polymer conjugates was carried out in cel-lophane membrane dialysis bags, and the in vitro release profiles were established separately in enzyme-free simulated gastric and intestinal fluids (SGF, pH 1 and SIF, pH 7.4). The detection of a hydrolysis solution by UV spectroscopy at selected intervals showed that the drug can be released by hydrolysis of the ester bond between the drug and polymer backbone at a low rate. Drug release studies showed that increasing the MAA content in the copolymer enhances the rate of hydrolysis in SIP. These results suggest that these polymeric prodrugs can be useful for the release of ibuprofen in controlled release systems.

황련해독탕 중 3종 생리활성 물질의 HPLC-DAD 동시 정량분석법 확립 (Simultaneous Analysis of three Marker Components in Hwangryunhaedok-tang by HPLC-DAD)

  • 양혜진;원진배;마진열;마충제
    • 약학회지
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    • 제55권1호
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    • pp.64-68
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    • 2011
  • In this study, a high performance liquid chromatography-diode array detector method was established, for simultaneous determination of three compounds, berberine, palmatine and geniposide in Hwangryunhaedok-tang, To develop and validate method, $C_{18}$ column (5 ${\mu}M$, 4.6 mm${\times}$250 mm) was used with gradient mobile phase, water containing 0.1% trifluoroacetic acid (TFA) and MeOH at the column temperature of $30^{\circ}C$. UV wavelength was set at 230 and 280 nm. Validation of the chromatography method was evaluated by linearity, precision and accuracy test. Calibration curve of standard components showed good linearity ($R^2$ > 0.9999). The limits of detection (LOD) and limits of quantification (LOQ) varied from 0.05 to 0.17 ${\mu}g/ml$ and 0.15 to 0.53 ${\mu}g/ml$, respectively. The relative standard deviations (RSDs) data of intra-day and inter-day test were in less than 2.99% and 1.90%, respectively. The results of the accuracy test were in the range of 98.36 to 102.52% with RSDs values 0.32 to 1.98%. The results of validation indicated that this method was a very accurate and sensitive assay.

Organopalladium(II) Complexes as Ionophores for Thiocyanate Ion-Selective Electrodes

  • Kim, Dong-Wan;Lee, So-Hyun;Kim, Jung-Hwan;Kim, Jin-Eun;Park, Jong-Keun;Kim, Jae-Sang
    • Bulletin of the Korean Chemical Society
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    • 제30권10호
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    • pp.2303-2308
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    • 2009
  • A thiocyanate poly(vinyl chloride) (PVC) membrane electrode based on [1,2-bis(diphenylphosphino)ethane]dihalopalladium( II), [(dppe)$PdX_2$, X = Cl ($L^1$), X = I ($L^2$)] as active sensor has been developed. The diiodopalladium complex, [(dppe)$PdI_2](L^2$) displays an anti-Hofmeister selectivity sequence: $SCN^-\;>\;I^-\;>\;{ClO_4}^-\;>\;Sal^-\;>\;Br^-\;>\;{NO_2}^-\;>\;{HPO_4}^-\;>\;AcO^-\;>\;{NO_3}^-\;>\;{H_2PO_4}^-\;>\;{CO_3}^{2-}$. The electrode exhibits a Nernstian response (-59.8 mV/decade) over a wide linear concentration range of thiocyanate ($(1.0\;{\times}\;10^{-1}\;to\;5.0\;{\times}\;10^{-6}$ M), low detection limit ($(1.1\;{\times}\;10^{-6}$ M), fast response $(t_{90%}$ = 24 s), and applicability over a wide pH range (3.5∼11). Addition of anionic sites, potassium tetrakis[p-chlorophenyl] borate (KTpClPB) is shown to improve potentiometric anion selectivity, suggesting that the palladium complex may operate as a partially charged carrier-type ionophore within the polymer membrane phase. The reaction mechanism is discussed with respect to UV-Vis and IR spectroscopy. Application of the electrode to the potentiometric titration of thiocyanate ion with silver nitrate is reported.