• Title/Summary/Keyword: Chromatographic analyses

Search Result 61, Processing Time 0.02 seconds

Analytical Methods for Phenolic Compounds in Water and Wastewaters(I) (Phenol류의 분석방법에 관한 연구(I))

  • 김낙주;신현진
    • Journal of Environmental Science International
    • /
    • v.7 no.6
    • /
    • pp.811-815
    • /
    • 1998
  • Currently in Korea, standard operating procedure for the analyses of phenolic compounds in water is the spectrometric comparison of colors developed by 4-amino antipyrin with phenolic compounds. It is however that this method cannot identify individual compound and that some phenolic compounds do not react with 4-amino antipyrin. Spectrometric determinations of phenolic compounds were compared with chromatographic analyses of gas chromatography (GC) and high pressure liquid chromatography (HPLC) of various phenolic compounds. Individual phenolic compounds could be determined by both chromatographic methods but HPLC methods were more precise with lower detection levels in general.

  • PDF

Theoretical Analysis of Chromatographic Peak Asymmetry and Sharpness by the Moment Method Using Two Peptides

  • Choi Du Young;Row Kyung Ho
    • Biotechnology and Bioprocess Engineering:BBE
    • /
    • v.9 no.6
    • /
    • pp.495-499
    • /
    • 2004
  • The analyses of peak shapes in chromatography are useful in operating chroma­tographic system. The asymmetry and sharpness of a chromatographic peak are estimated by the reversed-phase adsorption of two standard peptides (angiotensin II bradykinin) on $C_{18}$ In this work, the average particle diameters of $C_{18}$ were 5 and 15 $\mu$m, while the pore sizes were 100 and 300 A. The composition of the mobile phase was $50/50\;vol.\;{\%}$ of a binary mixture of acetonitrile and water with $0.1\%$ TFA, and the particles were packed in a stainless column ($4.6{\times}150$ mm). The third and the fourth central movement were calculated from the chromatographic elution curves by moment analysis. The peak asymmetry was determined by two theoretical calculations: the asymmetry factor by elution peak analysis and skewness with moment analysis. The sharpness was estimated by the fourth central moment. In this work, the most acceptable skewness was calculated when the pore size was 300 A. The large excess was observed on small pore size.

Composition and Evaluation of the Thermal Desorption-Gas Chromatographic System for the Measurement of Volatile Organic Compounds in Air (공기 중 휘발성 유기화합물의 측정을 위한 열탈착-분석시스템의 구성 및 평가)

  • 이수형;송희남;김희갑
    • Environmental Analysis Health and Toxicology
    • /
    • v.17 no.1
    • /
    • pp.63-71
    • /
    • 2002
  • The thermal desorption-gas chromatographic (TD-GC) system has been constructed for the measurement of volatile organic compounds. The thermal desortion unit is composed of four major parts: 1) the control part; 2) the thermal desorption part; 3) the focusing part; and 4) the injection part. The peltier element was introduced to the focusing part for the temperature of the focusing tube to reach-35$^{\circ}C$. The system was tested for the linearity of the calibration curves and reproducibility of instrumental analyses using some disinfection by-products (DBPs) and BTXs (benzene, toluene and p-xylene). The coefficients of determination (r$^2$) for all the calibration curves made were higher than 0.998, and the coefficients of variation (CV) for triplicate measurements were all within 10%. The system also has been tested for field applicability. The analysis of field samples showed that there was no breakthrough problem in the sampling system and that the system could be applied to field measurements.

Analyses of Flavor Qualities of Vegetable Oils by Gas Chromatography (가스크로마토그래피에 의한 식물성 기름의 향미품질의 분석)

  • Yoon, Suk-Hoo;Kim, Jong-Goon;Min, David B.
    • Korean Journal of Food Science and Technology
    • /
    • v.17 no.5
    • /
    • pp.355-360
    • /
    • 1985
  • Soybean, hydrogenated soybean and corn oils, which were exposed to fluorescent light for different periods of time, were evaluated for sensory qualities by subjective sensory evaluation and instrumental gas chromatographic analysis. Sensory evaluation was conducted in 8 laboratories using a 10-point hedonic scale with a total of 95 panel members. The correlation coefficients between sensory scores and predicted sensory scores by gas chromatographic analysis for the 8 laboratories varied from 0.10 to 0.99. However, most laboratories had better than 0.90, which was considered excellent. The correlation coefficients between sensory scores of the 95 panel members and predicted sensory scores using the amount of 2. 4-decadienal isomers in oil determined by a gas chromatographic method for soybean, hydrogenated soybean, and corn oils, were r=0.96, r=0.97, and r=0.97, respectively. The correlation study suggests that it is possible to obtain realistic results of oil flavor qualities from the instrumental evaluation by combining improved gas chromatographic analysis, sensory evaluation, and statistical analysis for practical purposes.

  • PDF

Metabolism of Dimethylphthalate by Aspergillus niger

  • Pradeepkmar;Sharanagouda;Karegoudar, T.B.
    • Journal of Microbiology and Biotechnology
    • /
    • v.10 no.4
    • /
    • pp.518-521
    • /
    • 2000
  • Aspergillus niger is capable of metabolizing dimethyphthalate. The maximum weight of mycelium wa observed afterabout 6-8 dys of incubation. A TLC analysis revealed the accumulation of metabolites in the resting cell culture. Monomethylphthalate, phthalate, and protocatechuate were shown to be the intermediates by thin layer chromatographic and spectrophotometric analyses. The fungus metabolized dimethylphthalate through monomethylphthalate, phthalate, and protocatechuate as evidenced by the oxygen uptake and an enzymatic analysis. The terminal aromatic metabolite, protocatechuate, is metabolized via the ortho-cleavage pathway.

  • PDF

Analyses of phenolics in cigarette smoke by GC-MS with the multiple ion selction technique

  • Park, Jeen-Woo
    • Archives of Pharmacal Research
    • /
    • v.5 no.2
    • /
    • pp.71-77
    • /
    • 1982
  • Improvements in the analytical methodology used in the gas chromatographic/mass spectral analysis of phenolic compounds from cigarette smoke are described. For the direct analysis of crude samples, pyridine extraction and the glass capillary column GC was used for the separation of phenolics as trimethylsilyl derivativatives. The separations of cigarette smoke on Carbowax 20M and SE-54 wall coated open tubular columns are given. Improved methodology for the routine quantitation of the identified components using the computer-controlled multiple ion selection technique of MS presented. Considerations pertaining to routine analyses of a multitude of complex smoke samples are also discussed.

  • PDF

Evaluation of Methods for Cyanobacterial Cell Lysis and Toxin (Microcystin-LR) Extraction Using Chromatographic and Mass Spectrometric Analyses

  • Kim, In S.;Nguyen, Giang-Huong;Kim, Sung-Youn;Lee, Jin-Wook;Yu, Hye-Weon
    • Environmental Engineering Research
    • /
    • v.14 no.4
    • /
    • pp.250-254
    • /
    • 2009
  • Contamination of microcystins, a family of heptapeptide hepatotoxins, in eutrophic water bodies is a worldwide problem. Due to their poisoning effects on animals and humans, there is a requirement to characterize and quantify all microcystins present in a sample. As microcystins are, for most part, intracellular toxins produced by some genera of cyanobacteria, lysing cyanobacterial cells to release all microcystins is considered an important step. To date, although many cell lysis methods have been used, little work has been conducted comparing the results of those different methods. In this study, various methods for cell lysis and toxin extraction from the cell lysates were investigated, including sonication, bead beating, freeze/thaw, lyophilization and lysing with TritonX-100 surfactant. It was found that lyophilization, followed by extraction with 75% methanol, was the most effective for extracting toxins from Microcystis aeruginosa cells. Another important step prior to the analysis is removing impurities and concentrating the target analyte. For these purposes, a C18 Sep-Pak solid phase extraction cartridge was used, with the percentage of the eluent methanol also evaluated. As a result, methanol percentages higher than 75% appeared to be the best eluting solvent in terms of microcystin-leucine-arginine (MC-LR) recovery efficiency for the further chromatographic and mass spectrometric analyses.

A NUMERICAL STUDY ON THE FLOW CHARACTERISTICS OF GAS CHROMATOGRAPHIC COLUMN (가스 크로마토그래픽 컬럼의 유동특성에 대한 수치적 연구)

  • Kim T.-A.;Kim Youn J.
    • 한국전산유체공학회:학술대회논문집
    • /
    • 2005.10a
    • /
    • pp.21-26
    • /
    • 2005
  • Gas Chromatography (GC) is a wisely technique used for the separation and analysis of liquid and gas sample. Separation of the sample vapors is achieved via their differential migration through a capillary column with an insert carrier gas. The identity and quantity of each vapor in the mixer can be determined from its retention time in the column and a particular property of the gas, such as thermal conductivity, which can be related to the concentration of sample vapor in the carrier gas. Therefore, the flow characteristics in the spiral gas chromatographic column are numerically investigated in this study. Especially, different pressure drop between the front and the rear of GC column with various flow rates is estimated the governing equations are derived from making using of three-dimensional Naver-Stokes equation with incompressible and laminar model due to the nature of low Reynolds number flow. Using a commercial code, FLUENT, the pressure and flow fields in GC column are calculated with various flow rates. The characteristics of thermal cycling which is one of the most important factors affecting the column efficiency and analysis time is also estimated. Furthermore, numerical analyses are also carried out by using commercial code, ANSYS, with various values of power, which is applied to the heating element located at lower GC column.

  • PDF

Chromatographic Selectivity of Cyano-Bonded Silica Columns in RPLC Based on the Linear Solvation Energy Relationships

  • Park, Jung-Hag;Jang, Myung-Duk;Kwon, Se-Mok
    • Bulletin of the Korean Chemical Society
    • /
    • v.13 no.1
    • /
    • pp.75-79
    • /
    • 1992
  • Differences in chromatographic properties in RPLC of four brands of cyano bonded silica stationary phases are rationalized in terms of the type and relative strength of the solute-stationary phase interactions, which can be readily inferred from multiple linear regression analyses of retention data for a set of standard compounds on the stationary phases under study based on the linear solvation energy relationships (LSERs). Although four brands of cyano bonded columns studied (CPS-Hypersil, Ultrasphere cyano, Spherisorb-CN and ${\mu}$-Bondapak-CN) have similar bonding density and have been prepared from monofunctional cyanopropylsilane reagents, they possess quite different, relative hydrogen bonding (HB) donor and acceptor strengths. Comparison of the retention behavior on a cyano-bonded silica column with that on an ODS column shows that there are significant differences in the strength of HB interactions between the solute and the stationary phase on the two columns with different functionalities. Information on the differences in the interaction characteristics among brands of the cyano-bonded silica columns and between the ODS and cyano-bonded columns can be utilized to optimize the selectivity for a given separation on these columns.

Quantitation of Mevinolinic Acid in Human Plasma by HPLC (고속액체크로마토그래피를 이용한 사람 혈장중 메비놀린 산의 정량)

  • Oh, Han-Suk;Park, Dong-Young;Seo, Sung-Hoon;Kim, Young-Gwan;Hong, Seon-Pyo;Choi, Young-Wook;Lee, Kyung-Tae
    • Journal of Pharmaceutical Investigation
    • /
    • v.30 no.4
    • /
    • pp.279-282
    • /
    • 2000
  • Simple and precise high-performance liquid chromatographic (HPLC) assay was developed and validated for the determination of a HMG-CoA reductase inhibitor, $lovastatin^{TM}$ and its active metabolite (mevinolinic acid) in human plasma. The method involved solid phase extraction of mevinolinic acid and internal standard using Sep-Pak Cartridge. Samples were analyzed by reversed-phase HPLC using $Capcell-Pak\;C_{18}$ column with ultraviolet detection at 238 nm. The quantitation limit of mevinolinic acid was 2 ng/ml and the calibration curve was linear over the range of 2-50 ng/ml $(r^2>0.999)$ with human plasma. The analyses of quality control samples indicated that the normal values could be predicted with an accuracy >97%. The intra- and inter-day coefficients of variation for the analyses were <10%. The average recoveries were similar (79%) for mevinolinic acid and methylmevinolinic acid. The method described has been successfully applied to the quantification of mevinolinic acid in about 1,000 human plasma samples over six-month period.

  • PDF