• Title/Summary/Keyword: fluorescence detector

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Pretreatment of Fish for the determination of polycyclic aromatic hydrocarbons using alkali digestion (알칼리분해를 이용한 어류 중 다환방향족탄화수소의 전처리방법)

  • Hu, Soojung;Lee, Hyomin;Chae, Youngzoo;Yoo, Eun-Ah
    • Analytical Science and Technology
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    • v.18 no.5
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    • pp.403-409
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    • 2005
  • Polycyclic Aromatic Hydrocarbons(PAHs) contamination arises from several sources including processing of food(smoking, direct drying, cooking) and environmental contamination of air, water, or soil, the later being considered as the most important. In this study, to establish the analytical method for some PAHs[benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene, indeno(1,2,3-c,d)pyrene] in fish, alkali digestion time, extraction solvents, elution volume of florisil cartridge for clean-up have been optimized. The methodology involved saponification and extraction with n-hexane, clean-up on Sep-Pak florisil cartridges and determination by HPLC/FLD(High Performance Liquid Chromatography/Fluorescence Detector). Overall method recoveries for 8 PAHs spiked into these products ranged from 90 to 106%.

Simultaneous Fluorimetric Determination of On-line Preconcentrated HANs, DCAD and TCAD by Using RPLC with a Postcolumn Derivatization System

  • Jung, Sung-Woon;Choi, Yong-Wook
    • Bulletin of the Korean Chemical Society
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    • v.34 no.6
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    • pp.1783-1790
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    • 2013
  • A simultaneous analytical method has been developed for the fluorimetric determination of haloacetonitriles (HANs) [dichloroacetonitrile (DCAN), trichloroacetonitrile (TCAN), dibromoacetonitrile (DBAN), haloacetamides [dichloroacetamide (DCAD), and trichloroacetamde (TCAD)] in drinking water by using the combined on-line perconcentration/reversed phase liquid chromatography (RPLC)-postcolumn detection system. This on-line perconcentration system was achieved by employing a precolumn packed with a commercial solid phase extraction (SPE) sorbent for the enrichment and purification of the target analytes. The haloacetonitriles and haloacetamides were separated on CN analytical column in a 7.5% methanol-0.02 M phosphate buffered mobile phase at pH 3. The column effluents were reacted with postcolumn reagents of ophthaldialdehyde (OPA) and sulfite ion at pH 11.5, to produce a highly fluorescent isoindole fluorophore, which were measured with a fluorescence detector. Under the optimized conditions for RPLC and the postcolumn derivatization system all of the coefficient of determination of the standard calibration curves for the target analytes were over 0.99 and had a linear range from 5 to 100 ${\mu}g/L$. The detection limits showed 1.6 ${\mu}g/L$ for DCAD, 0.1 ${\mu}g/L$ for TCAD, 0.6 ${\mu}g/L$ for DCAN, 1.6 ${\mu}g/L$ for TCAN and 1 ${\mu}g/L$ for DBAN, and the recoveries were ranged from 64 to 99% except for DCAD with precisions less than 4.9% in distilled water, and from 72(${\pm}4%$) to 116%(${\pm}2%$) in tap water.

Measurements of Polycyclic Aromatic Hydrocarbons(PAHs) Concentration in Air of the Seoul Underground Shopping Stores (서울시 지하상가 공기중 다환방향족 탄화수소의 농도조사에 관한 연구)

  • 전준민;김윤신
    • Journal of Korean Society for Atmospheric Environment
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    • v.9 no.1
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    • pp.81-92
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    • 1993
  • A purpose of this study was carried out to investigate the concentrations of four elements of PAHs(Polycyclic Aromatic Hydrocarbons) in suspended particulate matters of underground shopping stores in Seoul city. The particulate matters were collected at five underground shopping stores(Yongdungpo, Myongdong, Ulchiro, Express Terminal, Chamshil) in the Seoul area during February-October, 1992. Samples were collected using cascade impactor of low volumn air sampler and were analysed using High Performance Liquid Chromatography(HPLC) with fluorescence detector. Calibration on HPLC analyse is nearly accord with retention time between the standard solution and the samples. Analysed results obtained favorable analysing recovery rate of 97.3% and coefficient of variation of 1.60%. Mean concentrations of suspended particulate matters in five underground shopping stores wre 216.3 g/$m^3$ and observed higher at fine particles(117.2 g/$m^3$) which is respirable particulates than coarse particles(99.2 g/$m^3$). Concentrations of four species PAH were determined with anthracene of 16.8ng/$m^3$, fluoranthene of 72.3ng/$m^3$, benzo(a)pyrene of 0.54ng/$m^3$, and benzo(k)fluoranthene of 0.29ng/$m^3$, respectively. Fluoranthene levels were significantly higher than those levels in other components. PAHs concen-tration at shopping areas showed 21.3ng/$m^3$ in Yongdungpo, 35.1ng/$m^3$ in Myongdong, 23.4ng/$m^3$ in Ulchiro, 11.1ng/$m^3$ in Express Terminal, and 21.4ng/$m^3$ in Chamshil, respectively. Particularly, benzo(a)pyrene and benzo(k)-fluoranthene were detected over 83 percentage in fine particles, while fluoranthene wre highly detected in coarse particles. Also, higher concentrations of benzo(a)pyrene, benzo(k)fluoranthene were found in winter while levels of anthracene and fluoranthene were found higher in summer than other seasons.

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Water-Soluble Vitamins Contents in Seafood-Based Dishes (수산물 조리 식품에 함유된 수용성 비타민 함량)

  • Kim, Naeun;Kim, Younghwa
    • The Korean Journal of Food And Nutrition
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    • v.33 no.4
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    • pp.390-398
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    • 2020
  • The purpose of this study was to determine the contents of water-soluble vitamins B1 (thiamine), B2 (riboflavin), B3 (niacin) and B12 (cyanocobalamin) in seafood-based dishes by using the high-performance liquid chromatography with the ultra violet and fluorescence detector. The vitamin B1, B2, B3 and B12 contents were analyzed in 29 seafood-based dishes. The method validation was performed on the method to determine the linearity, accuracy, limits of quantification, limits of detection and precision for vitamin B1, B2, B3 and B12. An excellent linearity range (R2=0.999~1.000) in the calibration curve for the water-soluble vitamins was observed. All analytical methods for the water-soluble vitamins showed the acceptable accuracy (89.4~119.7% recovery) and the precision (0.6~4.8% repeatability and 1.0~4.2% reproducibility). The highest content of vitamin B1 was 2.646 mg/100 g in the kkongchi-jorim, and the highest contents of vitamin B2, B3 and B12 were 0.370 mg/100 g, 10.971 mg/100 g, and 17.193 ㎍/100 g, respectively, in the kkongchi-gui. Our results provide reliable data on the contents of the water-soluble vitamins of seafood-based dishes in Korea.

Bioequivalence of Sinil Atenolol Tablets to Tenormin Tablets (Atenolol 50 mg) (테놀민 정(아테놀올 50 mg)에 대한 신일아테놀올 정의 생물학적 동등성)

  • Gwak, Hye-Sun;Kang, Sung-Ha;Chun, In-Koo
    • Journal of Pharmaceutical Investigation
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    • v.33 no.1
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    • pp.51-53
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    • 2003
  • This study was conducted to compare the bioavailability of a generic product of Sinil Atenolol Tablets (Sinil Pharmaceutical Co., Ltd., Korea) with the innovator product, $Tenormin^{\circledR}$ Tablets in 20 healthy Korean volunteers. The volunteers received a single 50 mg dose of each atenolol formulation according to a randomized, two-way crossover design. Plasma samples were obtained over a 24-hour interval, and atenolol concentrations were determined by HPLC with a fluorescence detector. From the plasma atenolol concentration vs time curves, the following parameters were compared: area under the plasma concentration-time curve (AUC), peak plasma concentration $(C_{max})$, time to reach peak plasma concentration $(T_{max})$, and terminal first order elimination half-life $(t_{1/2})$. No statistically significant difference was obtained between the $T_{max}$ values, and the logarithmic transformed AUC and $C_{max}$ values of the two products. The 90% confidence for the ratio of the logarithmically transformed AUC and $C_{max}$ values of Sinil Atenolol Tablets over those of $Tenormin^{\circledR}$ Tablets were calculated to be between 0.99 and 1.07, and 1.04 and 1.16, respectively; both were within the bioequivalence limit of 0.80-1.25. The mean of $T_{max}$ in $Tenormin^{\circledR}$ Tablet group was 3.68 hour, and that in Sinil Atenolol Tablet group was 3.65 hour. The values of $t_{1/2}$ between the two products were found comparable, and the mean $t_{1/2}$ values of $Tenormin^{\circledR}$ Tablets and Sinil Atenolol Tablets were 5.9 and 6.0 hour, respectively. Based on these results, it was concluded that Sinil Atenolol Tablets were comparable to $Tenormin^{\circledR}$ Tablets in both the rate and extent of absorption, indicating that Sinil Atenolol Tablets were bioequivalent to the reference product, $Tenormin^{\circledR}$ Tablets

Bioequivalence of Bisoprolol Tablet (Bisoprolol hemifumarate 5 mg) (모노콜정에 대한 콩커정의 생물학적 동등성 평가)

  • Ko, In-Ja;Chi, Sang-Cheol
    • Korean Journal of Clinical Pharmacy
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    • v.14 no.2
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    • pp.85-90
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    • 2004
  • Bisoprolol, one of the $\beta_1-adrenorecepter$ antagonist, has been used for the treatment of mild to moderate essential hypertension anti stable angina pectoris. The oral bloavailability of bisoprolo1 is high $(90\%)$ and the drug has a long elimination half-life, $9{\sim}12\;hr$, which allows once-daily administration. The bioequivalence of two bisoprolol preparations was evaluated according to the guidelines of Korea Food & Drug Administration (KFDA). The test product was Concor $tablet^{(R)}$ made by Newgenpharm and the reference product was Monocor $tablet^{(R)}$ made by Wyeth Korea. Twenty healthy male subjects, 23.8 (21-30) years old and 03.8(52-92) kg, were randomly divided into two groups and a randomized $2\times2$ cross-over study was employed. After two tablets containing 10 mg bisoprolol hemifumarate were orally administered, blood was taken at predetermined time intervals and the concentration of bisoprolol in plasma was determined using an HPLC method with fluorescence detector. Two pharmacokinetic parameters, $AUC_t\;and\;C_{max}$ were calculated and analyzed statistical]y for the evaluation of bioequivalence of the two products. Analysis of variance was carried out using logarithmically transformed parameter values. The $90\%$ confidence intervals of $AUC_t\;and\;C_{max}$ were log $0.95{\sim}1og\;1.04\;and\;1og\;0.96{\sim}1og\;1.07,\;respectively.$ These values were within the acceptable bioequivalence intervals of log $0.8{\sim}log\;1.23$. Thus, the criteria of the KFDA guidelines for the bioequivalence was satisfied, indicating that Concor tablet is bioequivalent to Monocor tablet.

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Monitoring and Risk Assessment of Benzo(a)pyrene Content in Medicinal Herbs (유통 한약재 중 벤조피렌 함량 모니터링 및 안전성 평가)

  • Lee, Sae Ram;Kim, Ae Kyung;Kim, Sung Dan;Lee, Hyun Kyung;Lee, Hee Jin;Ryu, Hoe Jin;Lee, Jung Mi;Yu, In Sil;Jung, Kweon
    • Korean Journal of Pharmacognosy
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    • v.48 no.3
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    • pp.237-242
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    • 2017
  • In this study, to investigate of safety for Benzo(a)pyrene in medicinal herb, 8 kinds of selected commercial herbal medicines (Rehmanniae Radix, Rehmanniae Radix Preparata, Amomi Tsao-Ko Fructus, Cimicifugae Rhizoma, Cyperi Rhizoma, Magnoliae Cortex, Scutellariae Radix, Scrophulariae Radix) were analysed using the high performance liquid chromatography with fluorescence detector and assessed the health risk. The levels of benzo(a)pyrene were from non-detection to $28.1{\mu}g/kg$, and the average was $3.6{\mu}g/kg$. Based on a nationwide survey of the consumption of medicinal herb by the Korean population, we estimated the potential risk from the ingestion of benzo(a)pyrene. The estimated daily intake of benzo(a)pyrene was 1.6 ng/kg b.w./day for group only know the daily average intake of medicinal herb. The MOE (margin of exposure) of benzo(a)pyrene for estimate of health risk was $1.93{\times}10^5$. Therefore, health risk from benzo(a)pyrene through intake of herbal medicine was considered negligible.

Interpretation of the Chemical Transformation of Individual Asian Dust Particles Collected on the Western Coast of Korean Peninsula

  • Ma, Chang-Jin;Kim, Jong-Ho;Kim, Ki-Hyun
    • Asian Journal of Atmospheric Environment
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    • v.6 no.1
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    • pp.14-22
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    • 2012
  • This paper is focused on the comprehensive and detailed interpretation for the chemical transformation of individual Asian dust (hereafter called "AD") particles during long-range transport from source regions to receptor area. A multi-stage particle sampler was operated at a ground-based site in Taean, Korea directly exposed to the outflow of air masses from China during AD period in April 2003. Both quantitative and qualitative analyses for size-classified individual particles were carried out by a microbeam X-ray fluorescence (XRF) method and a microbeam Particle Induced X-ray Emission (micro-PIXE), respectively. Among major characteristic elements, the elemental masses of soil derived components, sulfur, and chloride varied as a function of particle size showing the monomodal maximum with a steeply increasing at 3.3-4.7 ${\mu}m$ particle size. Although the details on chemical composition of AD particle collected on a straight line from source area to our ground-based site are needed, a large amount of Cl coexisted in and/or on AD particles suggests that AD particles collected in the present study might be actively engaged in chemical transformation by sea-salt and other Cl containing pollutants emitted from the China's domestic sources. Through the statistical analyses it was possible to classify individual AD particles into six distinct groups. The internally mixed AD particles with Cl, which has various sources (e.g., sea-salt, coal combustion origin HCl, gaseous HCl derived from the adsorption of acids to sea-salt, and Cl containing man-made particles) were thoroughly fractionated by the elemental spectra drivened by the double detector system of micro-PIXE.

Determination of Glutathione in Biological Samples by Ion-pairing HPLC/FLD (이온쌍 HPLC/FLD를 이용한 생체 시료중의 Glutathione 농도 분석)

  • Yoo, Jeong-Yeon;Lee, Kyoung-Ok;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.12 no.1
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    • pp.28-33
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    • 1999
  • Glutathione(GSH) in biological samples was determined by high performance liquid chromatographic(HPLC) method with fluorescence detector(FLD) after monobromobimane(MBB) or 4-fluoro-7-sulfobenzofurazan(SBD-F) derivatization. The detection limit of $0.03{\mu}g/mL$ was obtained after MBB derivatization, derivative of MBB was about 200 times more sensitive than that of SBD-F. N-acetylcysteine was used as internal standard and tetrabutylammonium ion as counter ion for better separation. The determination by ion-pairing chromatography after MBB derivatization was characterized by linearity in the range between $0.08{\sim}8.33{\mu}g/mL$ with a good correlation coefficient of 0.998. By precision test appeared relative standard deviation at less than 5% at three different concentrations. This method can be used for the analysis of GSH in plasma and tissue.

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Plasma total homocysteine and macrovascular complications are associated with food and nutrient intake in patients with Type II diabetes mellitus

  • Chang, Nam-Soo;Kim, Ji-Myung;Kim, Hye-Sook;Cho, Yong-Wook
    • Nutrition Research and Practice
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    • v.1 no.2
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    • pp.79-83
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    • 2007
  • The present study was conducted to document the association between plasma homocysteine levels and the presence of macrovascular angiopathy with food and nutrient intake patterns among patients with Type II diabetes mellitus in Korea. Plasma total homocysteine concentration was analyzed by HPLC-fluorescence detector method in 127 patients with non-insulin dependent diabetes mellitus. Logistic regression analyses were performed respectively to study the association of plasma homocysteine levels with clinical and dietary characteristics and macroangiopathy (MA). The average plasma homocysteine level of patients with MA was $14.2{\mu}mol/l$, which was significantly higher than that of patients without MA ($11.4{\mu}mol/l$). The proportions of patients with MA showed a significant difference, being 32.3% in hyperhomocysteinemic ($>14.0{\mu}mol/l$) patients and 13.5% in others with homocysteine levels lower than $14.0{\mu}mol/l$. Odds ratios for macroangiopathy by tertile increase of plasma homocysteine concentration were 1.633 ($Q_2$) and 4.831 ($Q_3$), when adjusted for age, sex, and cigarette smoking. Patients with MA consumed reduced amounts of vitamin $B_1,\;B_2$, and folate. The results indicate that the plasma homocysteine levels are significantly increased in NIDDM patients who have macroangiopathy. Dietary management such as increased fruits and vegetables and decreased potatoes and starches might be beneficial for the prevention of macroangiopathy in diabetic patients.