• Title/Summary/Keyword: Spectrofluorometric determination

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Spectrofluorometric determination of caffeine using acridine orange-β-cyclodextrin inclusion complex (Acridine orange-β-cyclodextrin 내포 착물을 이용한 카페인의 분광형광법 정량)

  • Park, Jong Hee;Choi, Hee-Seon
    • Analytical Science and Technology
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    • v.26 no.6
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    • pp.353-356
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    • 2013
  • A method on the determination of caffeine in beverage with acridiene orange-${\beta}$-cyclodextrin (CD) inclusion complex was developed. The conditions such as pH of the sample solution and concentration of acridine orange and ${\beta}$-CD were optimized to 12.0(${\pm}0.5$), $1.9{\times}10^{-6}M$ and $1.25{\times}10^{-3}M$, respectively. Under these optimum conditions, the calibration curve of caffeine was obtained over concentration range of $5{\times}10^{-5}{\sim}1.1{\times}10^{-3}M$. The detection limit was $1.0{\times}10^{-5}M$. The relative errors(%) in beverage samples were less than 5.0%.

Determination of Heparin Using Norfloxacin-cerium Complex as a Fluorescence Probe by Spectrofluorimetry

  • Patil, Shailaja R.;Mote, Umesh S.;Patil, Shivajirao R.;Kolekar, Govind B.
    • Bulletin of the Korean Chemical Society
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    • v.30 no.12
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    • pp.3034-3038
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    • 2009
  • A simple, rapid, practical and sensitive spectofluorimetric method was developed for the determination of trace amount of heparin (Hep). Under the Optimum conditions, we studied the interaction between NFLX-Ce$^{3+}$-Hep complex by using absorption and fluorescence spectra. It was observed that Hep remarkably enhance the fluorescence intensity of the NFLX-Ce$^{3+}$ complex at ${\lambda}$= 356 nm in the buffer solution of pH = 7.60 and the enhancement effect is shown to relate with the concentration of Hep. The linear range and detection limit for the determination of Hep was obtained. By the Rosenthal graphic method, the association constant (K) and binding numbers (N) of Hep with probe were investigated. This method is relatively free of interference from coexisting substances and successfully applied for the determination of heparin in heparin sodium injection samples. A suitable mechanism of fluorescence enhancement between NFLX-Ce$^{3+}$ and the NFLX-Ce$^{3+}$-Hep systems were proposed and discussed.

Spectrofluorimetric Determination of n-Octanol Based on its Ternary Complex with $Eu^{3+}$ and TTA ($Eu^{3+}$, TTA, 그리고 n-Octanol의 삼성분착물에 의한 n-Octanol의 분광형광분석법에 관한 연구)

  • Cha, Ki-Won;Park, Kwang-Won
    • Analytical Science and Technology
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    • v.10 no.6
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    • pp.433-438
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    • 1997
  • The enhancing effect of n-octanol on the fluorescence intensity of the $Eu^{3+}$-thenoyltrifluoroacetone(TTA) system in the presence of Triton X-100 was studied using spectrofluorometric method. This complex exhibited very intense $Eu^{3+}$ ion fluorescence at 619nm, when optically excited at 345nm. Optimum conditions for the determination of n-octanol have also been investigated. The calibration graph was linear over the range $1{\times}10^{-5}M{\sim}1{\times}10^{-7}M$ and the detection limit for n-octanol is $1{\times}10^{-9}M$. The result obtained in the analysis of the synthetic sample agreed with the known value in the error range and the relative standard deviation was ca. 3.5%.

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Europium-Enoxacin Complex as Fluorescence Probe for the Determination of Folic Acid in Pharmaceutical and Biological Samples

  • Alam, Al-Mahmnur;Kamruzzaman, Mohammad;Lee, Sang-Hak;Kim, Young-Ho;Min, Kyung
    • Bulletin of the Korean Chemical Society
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    • v.33 no.9
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    • pp.3055-3060
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    • 2012
  • A simple, rapid and sensitive spectrofluorometric method was developed for the determination of folic acid (FA), based on its quenching effect on the fluorescence intensity of enoxacin (ENX)-europium ($Eu^{3+}$) complex as a fluorescent probe. Fluorometric interaction between ENX-$Eu^{3+}$ complex and FA was studied using UV-visible and fluorescence spectroscopy. The quenched fluorescence intensity at an emission wavelength of 614 nm was proportional to the concentration of FA. Optimum conditions for the determination of FA were investigated. Under optimal conditions, the reduced fluorescence intensity at 614 nm was responded linearly with the concentration of FA. The linearity was maintained in the range of $1.25{\times}10^{-9}$ to $1.50{\times}10^{-7}$ M (R = 0.9986) with the limit of detection ($3S_b/m$) (where $S_b$ is the standard deviation of blank and m is the slop of linear calibration curve) of $6.94{\times}10^{-10}$ M. The relative standard deviation (RSD) for 9 repeated measurements of $1.0{\times}10^{-9}$ M FA was 1.42%. This method was simple, cost effective, and relatively free of interference from coexisting substances. Successful determinations of FA in pharmaceutical formulation and biological samples with the developed method were demonstrated.

Studies on Benzo(a)pyrene Content in the Surface Soil of Seoul City (서울市 土砂中 Benzo (a) pyrene의 含量에 關한 硏究)

  • 孫東憲;金載翰
    • Journal of Korean Society for Atmospheric Environment
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    • v.5 no.2
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    • pp.12-20
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    • 1989
  • Distribution of benzo(a)pyrene (BaP) in Seoul surface soils was investigated with a simple micro-analytical method consisting of ultrasonic extraction, one-dimensional dual band thin-layer chromatographic separation (TLC) and spectrofluorometric determination. The TLC was done in the following condition: thin-layer plate; Kieselguhr G/Acetylated cellulose, Developer; 1st; ether, 2nd; methanol-ether-water (4:4:1, V/V). The results thus obtained were as follows; 1. All the samples collected from various areas were contained detectable amount of benzo(a)pyrene. The range and average of benzo(a)pyrene contents in Seoul areas are 0.20 $\sim$5.90ppm and 1.01 ppm, respectively. 2. Benzo(a)pyrene contents in soils obtained from commercial areas were much higher than those in industrial and residential areas. The contents range in commercial, industrial, and residential areas are 0.31 $\sim$ 5.90 ppm, 0.36 $\sim$ 1.22 ppm and 0.20 $\sim$ 0.67 ppm, respectively. 3. Benzo(a)pyrene contents in soils from major roads were far higher than those from side or park roads. The ranges of benzo(a)pyrene contents in major, park and side road are 0.40 $\sim$ 5.9 ppm, 0.20 $\sim$ 0.70 ppm, 0.31 $\sim$ 1.30 ppm, respectively. These findings suggest strongly that surface soils in Seoul city are polluted by benzo(a)pyrene probably emitted automobiles.

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Ion Exchange Separation and Spectrofluorometric Determination of Lanthanides in Nuclear Grade Material (이온 질환수지 및 형광분석법에 의한 핵급물질 중희토류원소의 분리정량)

  • Ki-Soo Cho;In-Suck Suh
    • Nuclear Engineering and Technology
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    • v.15 no.2
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    • pp.142-148
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    • 1983
  • Distribution coefficients between cation exchange resin (Dowex 50W$\times$8) and $\alpha$-hydroxyisobutric acid ($\alpha$-HIBA) are measured in order to separate traces of Sm, Eu, Gd and Dy from nuclear material. Individual separations are performed by pH gradient technique with 0.40M $\alpha$-HIBA from 3.40 to 3.60 in cation exchange resin after a group separation. Each of separated elements is determined with a fluorometric method except Gd by colorimetry. The results are applied to analyze Sm, Eu, Gd and Dy in magnesium diuranate (yellow cake).

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Determination of Terazocin in Human Plasma by Liquid Chromatography and Bioequivalence Study of Teratonin® Tablets (액체크로마토그래프법에 의한 사람 혈장 중 테라조신의 정량 및 테라토닌® 정의 생물학적 동등성)

  • Cho, Eun-Sook;Kang, Sung-Ha;Chun, In-Koo
    • Journal of Pharmaceutical Investigation
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    • v.32 no.2
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    • pp.119-125
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    • 2002
  • A rapid, selective and reproducible high-performance liquid chromatographic method has been developed for the determination of terazocin in human plasma. Terazocin plus the internal standard, prazocin hydrochloride, were extracted from alkalified plasma with tert-butylmethyl ether, back-extracted into 0.05% phosphoric acid. Fifty ${\mu}l-portions$ of extract were injected onto a octadecylsilane column and eluted with a mixture of acetonitrile, water and triethylamine (30 : 70 : 0.1 v/v, adjusted to pH 5.0 with dilute phosphoric acid) at a flow rate of 1.0 ml/min. The fluorescence intensity of column eluents was monitored at excitation wavelength of 250 nm and emission wavelength of 370 nm. No interference peaks were observed. The practical limit of quantitation was 5 ng/ml for terazocin. The average intraday and interday coefficients of variation were 4.15 and 3.54%, respectively. Also intraday and interday precisions over the range $5{\sim}60\;ng/ml$ were $0.49{\sim}2.92\;and\;0.38{\sim}5.12%$, respectively. The bioequivalence of two terazosin tablets, the $Hytrine^{\circledR}$ (Il Yang Pharmaceutical Co., Ltd.) and the $Teratonin^{\circledR}$ (Sam-A Pharmaceutical Co., Ltd.), was evaluated according to the guideline of Korea Food and Drug Administration (KFDA). Sixteen healthy male volunteers $(24.6{\pm}2.0\;years\;old)$ were divided into two groups and a randomized $2{\times}2$ cross-over study was employed. After one tablet containing 2 mg of terazosin was orally administered, blood was taken at predetermined time intervals and the concentration of terazosin in plasma was determined with a HPLC method using spectrofluorometric detector. AUC was calculated by the linear trapezoidal method. $C_{max}\;and\;T_{max}$ were compiled from the plasma drug concentration-time data. Analysis of variance (ANOVA) was utilized for the statistical analysis of the parameters. The results showed that the differences in $AUC_t,\;C_{max}\;and\;T_{max}$ between the two preparations were 0.21 %, 5.53% and 8.82%, respectively. The powers $(1-{\beta})\;for\;AUC_t,\;C_{max}\;and\;T_{max}$ were >99%, 97.49%, and 33.26%, respectively. Minimum detectable differences $({\Delta},\;%)\;at\;{\alpha}=0.1\;and\;1-{\beta}=0.8$ and the 90% confidence intervals were all less than ${\pm}20%$ except for $T_{max}.\;AUC_t\;and\;C_{max}$ met the criteria of KDFA for bioequivalence, indicating that $Teratonin^{circledR}$ tablets are bioequivalent to $Hytrine^{circledR}$ tablets.