• Analytical Science and Technology
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• v.16 no.5
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• pp.349-357
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• 2003

The universality of low molecular weight metabolites (i.e. amino acids, steroid hormones) allows rapid and straightforward investigation of biochemistry of genetically un-characterized species. Thus in vivo metabolic profiling of amino acid in combination with multivariate data analysis (metabolomics) offers great potential in comparative biology. In this paper, amino acid profiles in biological fluid (media) were studied by using HPLC/FLD. HPLC procedure for amino acids require the formation of derivatives due to the low absorption of the free compounds. o-Phthalaldehyde (OPA) used in association with a thiol, such as 3-mercaptopropionic acid (3-MPA), is one of the most popular and sensitive reagents, which yield quickly fluorescent iso-indoles at room temperature. To improve unstability of OPA/3-MPA derivatization, we optimized injector programs for fixed injection times. Linear regressions for the standard curves were linear in the range 0.5 - 100.0 ppb, giving correlation coefficents above 0.99. The detection limit were 1.70 pmol(GLU) - 23.81 pmol(SER). It is practically useful when the amount of sample is very low on single cells.

• Analytical Science and Technology
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• v.12 no.4
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• pp.318-325
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• 1999

Sludges from the wastewater of hanji production were analysed to see that sludges from the bleaching process, the bleach washing process, and the paper preparation process were fibrous, while sludges from the process cooking with NaOH and the process of final chemical and microbiological treatment were non-fibrous. Sludge solution from the bleaching process had the most amount of solid matters. Sludges from the bleaching process, the bleach washing process, and the final chemical and microbiological treatment process contained about 80-90 %(w/w) moisture. Owing to hypochlorite ion, pH of sludge from the bleaching process was higher than any other sludge samples. The inorganic components of sludges were determined by ICP-AES. The major inorganic component of sludge from the process cooking with NaOH was Na, while the sludge from the bleaching process had Na and Ca, major components in the final chemical and microbiological treatment process were Ca and Al. Trace amount of Mg, Fe, K, P, Mn and Ti were observed in sludges. Sludge from the bleaching process had ashes more than any other sludges. Shape of sludges observed by SEM was appeared to fibrous or crystalline, and the breadth of fibrous sludge was $5{\sim}50{\mu}m$. The sludge from the bleaching process had the most amount of matters soluble by cold and hot water and by alcohol-benzene.

• Analytical Science and Technology
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• v.12 no.3
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• pp.190-195
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• 1999

The metabolism of testosterone ($17{\beta}$-hydroxy-androst-4-en-3-one) was confirmed in horse after a single intramuscular administration of testosterone cypionate (750 mg). Solvent extracts of urine obtained with enzymatic hydrolysis and methanolysis were analyzed by GC/MS after oxime t-butyldimethylsilyl (oxime-TBDMS) derivatization. The structures of four urinary metabolite after testosterone administration in horse were determined based on EI mass spectra and $5{\alpha}$-androstane-$3{\beta}$, $17{\alpha}$-diol and $5{\alpha}$-androstane-$3{\beta}$-ol-17-one as major was confirmed with authentic standard. Also the concentrations of $5{\alpha}$-androstane-$3{\beta}$, $17{\alpha}$-diol, $5{\alpha}$-androstane-$3{\beta}$, $17{\beta}$-diol, dehydroepiandrosterone (DHEA), $5{\alpha}$-androstane-$3{\beta}$-ol-17-one and testosterone were determined in the urine of normal subjects and the urine after administration. The recovery and detection limit in the most drugs were 86.3~94.7% and 1~3 ppb, respectively. Correlation coefficients for calibration were in the range of 0.984~0.999. Excretion profile of testosterone presents the rapid and large increasement up to maximum values at days 5 after administration and the slow regression. The relative ratios of testosterone, its metabolites over DHEA were determined for indication of testosterone administration in horse doping.

• Analytical Science and Technology
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• v.11 no.3
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• pp.179-188
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• 1998

The capacity factor of fifteen phenol derivatives was determined with respect to the concentration of ${\alpha}$- or ${\beta}$-cyclodextrin [CD], the type as well as the content of organic solvent in the mobile phase, and the temperature. The effect of the inclusion complex formation between solutes and ${\alpha}$- or ${\beta}$-cyclodextrin on their retention and selectivity has been investigated. The inclusion effect of ${\beta}$-cyclodextrin was the most effective in aqueous methanol, whereas only a poor effect was observed in aqueous tetrahydrofuran and aqueous acetonitrile. A plot of the reciprocal of the capacity factor against $[CD]_T$ gives a straight line and the dissociation constant, $K_D$ of the inclusion complex can be calculated from the slope. It was possible to estimate the $k_D$ values in 100% water from a linear plot of $pK_D$ vs. water content in the solution by extrapolation. The separation factor, ${\alpha}$, of two compounds has been found to be affected not only by the $[CD]_T$ but also by their $K_D$ values. Under optimum conditions, some mixtures of phenol derivatives were able to separate successfully.

• Analytical Science and Technology
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• v.16 no.6
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• pp.488-498
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• 2003

By LC/MS/MS, the analytical method of sildenafil and its analogues (homosildenafil, vardenafil and tadalafil) used as used medical treatment of impotence was established. electrosprary ionization (ESI) and atmospheric pressure chemical ionization (APCI) as a ionization method were applied. Several parameter were varied and the sensitivity and reproducibility were compared. In LC/ESI-MS method, capillary voltage, cone voltage, extractor, entrance and RF lens to create appropriate productr ions for multiple reaction monitoring (MRM) were variable parameter, but the formation of the other product ions except the precursor ion could not detect. And the value of entrance, collision energy, exit, corona voltage, cone voltage, extractor, RF lens, cone gas, and desolvation gas in APCI mode were varied, only the creation pattern of fragment ions by the change of RF lens value were detected, and the limit of detection was decreased due to the increase of S/N. Ten millimole ammonium formate (pH 4.8):acetonitrile=70:30 by isocratic elution in HPLC system was shown the maximum sensitivity in MS, the detection limit of sildenafil, homosildenafil, vardenafil and tadalafil obtained by ESI-MRM were 0.10, 0.025, 0.025, and $0.25{\mu}g/mL$ at S/N>5, respectively.

• Analytical Science and Technology
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• v.16 no.6
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• pp.475-482
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• 2003

Uncertainty of final measurement results considering main uncertainty sources being in dioxin analysis of a blood sample was estimated. 'The Guide to the Expression of Uncertainty in Measurement' was suggested for accomplishment of this study. After uncertainties for the 11 compounds detected in this experiment of the 17 target compounds of dioxin and furan were calculated considering the uncertainty sources of each step, uncertainty for the total dioxin concentration was estimated by combining these values. The concentration of dioxin in blood sample was expressed as $0.0746{\pm}0.0074pg$ I-TEQ/g weight or $20.68{\pm}2.04pg$ I-TEQ/g lipid, including the uncertainty values obtained in this way. The former expression indicates the conversion concentration into the sample weight and the latter one indicates the conversion concentration into the lipid weight. The quality of measured analytical results could be assured quantitatively by estimating uncertainty of measurement results and showing the range of measurand.

• Analytical Science and Technology
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• v.10 no.6
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• pp.439-444
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• 1997

Twelve kinds (1set) standard materials of chemical ingredients of lead zirconate titanate[$Pb(ZrTi)O_3$] have been developed in order to determine fast and accurate measurement of X-ray fluorescence spectrometry. Especially, we used diluted(ahout sixteen times) filling compound($Li_2B_4O_7/LiBO_2=4/1$) to consider removal effect of matrix, storage convenience, and homogenous characteristics. As a result from the four different laboratories, we obtained extremly good agreement about the standard curve on twelve standard materials which containing eleven elements, PbO, $ZrO_2$, $TiO_2$, SrO, $WO_3$, $La_2O_3$, $Cr_2O_3$, MgO, $Nb_2O_5$, and $MnO_2$. The correlation factor of standard curve was over 0.998. However, ZnO has relatively low correlation factor, 0.977, because the concentration was 10ppm lower than other original materials. This analysis reveals that ZnO has shown the poor linearity as well as low fluorescence intensity. In present work, XRF standard materials are useful for determining a rapid and accurate results for major and minor elements concentration among PZT.

• Analytical Science and Technology
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• v.31 no.1
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• pp.23-30
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• 2018

Twenty-two allergy-induced aromatics in children were analyzed using a gas chromatography flame ionization detector (GC-FID) and gas chromatography mass spectrometer (GC-MSD). Analytes were extracted using an automatic Soxhlet extractor and centrifuged for 10 min in a fast freezing centrifuge, and the supernatant was transferred into a 2 mL vial and injected in split mode. Under the established conditions, the calibration curve showed linearity with a correlation coefficient of 0.996 or more. A wide range of sensitivity of 6.7 to 1,859,839 depending on the device characteristics and detector used was shown. The detection limit of the device was 0.0032 to $0.0335{\mu}g/mL$, and the maximum detection limit was less than $0.1{\mu}g/mL$. The detection limit of the method ranged from 0.0033 to $0.1161{\mu}g/mL$. In addition, the limit of quantification ranged from 0.0100 to $0.5422{\mu}g/mL$, with a level of precision ranging from 0.21 % to 4.89 % and a degree of accuracy ranging from 89 % to 111 %. The analytical method developed in this study was applied to commercial products.

• Analytical Science and Technology
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• v.31 no.1
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• pp.39-46
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• 2018

Carbaryl and seven organophosphorous pesticides were analyzed simultaneously using on-line solid phase extraction (on-line SPE) coupled with liquid chromatography tandem mass spectrometry (LC/MS/MS). The target pesticides are Carbaryl, Methyl demeton, Fenitrothion, Malathion, Parathion, Phenthoate, Diazinon, and EPN. This method includes the direct injection of $500{\mu}L$ in the water sample, a 15 min separation period using a rapid resolution liquid chromatography system with on-line SPE, and detection through electrospray ionization (ESI) positive mode. The percentage of recovery of all pesticides ranged from 85.3 % to 100 %. This method showed an accuracy of ${\geq}90.0%$, possessing limits of detection and quantification within 0.05 to $0.28{\mu}g/L$ and 0.16 to $0.89{\mu}g/L$, respectively. The correlation coefficients (r) for the calibration curves within a range of 0.5 to $8.0{\mu}g/L$ were higher than 0.99. The evaluation results showed the efficacy of the method for all contents, and no pesticides were detected in the water quality sample.

• Journal of Conservation Science
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• v.25 no.3
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• pp.245-256
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• 2009

Stereo-Microscope observation, ultrasonic velocity, shore hardness and standard color measurement performed for studies of physical characterization of Namsan granite after treated with consolidants. The consolidants used in experiment are 35wt% Silicate Nonparticle/100%1T1G (Nonparticle), 3%POSS-SO1455/97%1T1G(3%POSS1455), POSS-SO1458/97%1T1G (3%POSS1458), 3%7nm/97%1T1G(3%7nm), 3%16nm/97%1T1G(3%16nm), 3% 40nm/97%1T1G(3%40nm) develop with Sejong university, and Wacker Silres BS OH-100, Unil Sandsteinfestiger OH-100. The color of rock surface is darker than original one but similar to original samples with time, and ultrasonic velocity and shore hardness increased with after consolidant treatment.