Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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2001.06a
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pp.2111-2111
/
2001
A chemoinfometrical method for evaluating the quantitative determination of crystallinity one polymorphs based on fourie-transformed near-infrared (FT-NIR) spectroscopy was established. A direct comparison of the data with the ones collected from using the and compared with the conventional powder X-ray diffraction method was performed. [Method] The pPure a and g forms of indomethacin (IMC) were prepared by reportedusing published methods. Six kinds of standard samples obtained by physically mixing of a and g forms. After the powder X-ray diffraction profiles of samples have been measured, the intensity values were normalized to against the intensity of silicon powder as the as an external standard. The calibration curves for quantification of crystal content were based upon the total relative intensity of four diffraction peaks from of the form g crystal. FT-NIR spectra of six calibration sample sets were recorded 5 times with the NIR spectrometer (BRAN+LUEBBE). Chemoinfometric analysis was performed on the NIR spectral data sets by applying the principal component regression (PCR). [Results] The relation between the actual and predicted polymorphic contents of form g IMC measured using by the X-ray diffraction method shows a good straight linen linear relation., and it has slope of 0.023, an intercept of 0.131 and a correlation coefficient of 0.986. PCR analyses wereis was performed based on normalized NIR spectra sets offer standard samples of known content of IMC g form. IMC. A calibration equation was determined to minimize the root mean square error of the predictionthe prediction. Figure 1 shows a plot of the calibration data obtained by NIR method between the actual and predicted contents of form g IMC. The predicted values were reproducible and had a smaller standard deviation. Figure 2 shows that the plot for the predicted transformation rate (%) of form a IMC to form g as measured by X-ray diffractomeoy against to those as measured by NIR method. The plot has a slope of 1.296, an intercept of 1,109, and a correlation coefficient of 0.992. The line represents a satisfactory correlation between the two predicted values of form g IMC content. Thus NIR spectroscopy is an effective method for the evaluation to the pharmaceutical products of quantitative of polymorph.
Glucuronidation by the uridine diphosphateglucuronosy-ltransferase 1A enzymes (UGT1As) is a major pathway for elimination of particular drugs and endogenous substances, such as bilirubin. We examined the relation of eight single nucleotide polymorphisms (SNPs) and haplotypes of the UGT1A gene with their clinical factors. For association analysis, we genotyped the variants by direct sequencing analysis and polymerase chain reaction (PCR) in 218 healthy Koreans. The frequency of UGT1A1 polymorphisms, -3279T>G, -3156G>A, -53 $(TA)_{6>7}$, 211G>A, and 686C>A, was 0.26, 0.12, 0.08, 0.15, and 0.01, respectively. The frequency of -118 $(T)_{9>10}$ of UGT1A9 was 0.62, which was significantly higher than that in Caucasians (0.39). Neither the -2152C>T nor the -275T>A polymorphism was observed in Koreans or other Asians in comparison with Caucasians. The -3156G>A and -53 $(TA)_{6>7}$ polymorphisms of UGT1A were significantly associated with platelet count and total bilirubin level (p=0.01, p=0.01, respectively). Additionally, total bilirubin level was positively correlated with occurrence of the UGT1A9-118 $(T)_{9>10}$ rare variant. Common haplotypes encompassing six UGT1A polymorphisms were significantly associated with total bilirubin level (p=0.01). Taken together, we suggest that determination of the UGT1A1 and UGT1A9 genotypes is clinically useful for predicting the efficacy and serious toxicities of particular drugs requiring glucuronidation.
Korean Journal of Agricultural and Forest Meteorology
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v.5
no.3
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pp.200-207
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2003
'||'||'||'&'||'||'||'quot;Overheating index'||'||'||'&'||'||'||'quot;, the normalized difference in incident solar energy between a target surface and a level surface, is helpful in estimating the spatial variation in daily maximum temperature at the landscape scale. It can be computed as the ratio of the 4-hour cumulative solar irradiance surplus or deficit from that over a level surface to the maximum possible deviation (15 MJ $m^{-2}$ ) during the midafternoon. Ecosystem models may, for simplicity, use an empirical proxy (exposure index) variable combining slope and aspect in place of the overheating index to account for the variation of midafternoon solar irradiance. A comparative study with real-world landscape data was carried out to evaluate the performance of exposure index in replacing the overheating index. Overheating indices for summer solstice, fall equinox and winter solstice were calculated at 573,650 grid cells constituting the land surface of Donggye-Myun, Sunchang County in Korea, based on a 10-m DEM. Exposure index was also calculated for the same area and fitted for the variation of overheating index to derive a 2$^{nd}$ -order linear regression equation. The coefficient of determination ($R^2$) was 0.50 on summer solstice, 0.56 on fall equinox, and 0.44 on winter solstice, respectively. These are much lower than the theoretically calculated $R^2$ values ranging from 0.7 in summer to 0.9 in autumn. According to our study, exposure index failed to accurately predict the cumulative solar irradiance over a complex terrain, hindering its application to daily maximum temperature estimation. We suggest direct calculation of the overheating index in preference to using the exposure index.
The quantitative methods for the assessment of the cerebral blood flow using $^{99m}Tc$-HMPAO brain SPECT utilize the measured count distribution in some specific reconstructed tomographic slice or in algebraic summation of a few neighboring slices, rather than the true volumetric distribution, to estimate the relative regional cerebral blood flow, and consequently produce the biased estimates of the true regional cerebral blood flow. This kind of biases are thought to originate mainly from the arbitrarily irregular shape of the cerebral region of interest(ROI) which are analyzed. In this study, a semi-automated method for the direct quantification of the volumetric regional cerebral blood flow estimate is proposed, and the results are compared to those calculated by the previous planar approaches. Bias factors due to the partial volume effect and the uncertainty in ROI determination are not considered presently for the methodological comparison of planar/volumetric assessment protocol.
A series of experiments were conducted on procedures of $N_2$ fixation measurements with soybean (Glycine max. L.) root nodules by acetylene reducing assay and estimation of amounts of $N_2$ fixed by soybean root nodules grown in the pot. The results are summarized as follows; 1. In case of nitrogen fixing activities were determined by means of acetylene reducing method, more appropriates results were obtained with direct determination of root nodules which was adhering from root under 2 hours after incubation, while more fluctuated data was obtained with root nodules determined under separated conditions. 2. The weight of soybean nodules was linearly increased from 17 days to 55 days after planting, whereas, the amounts of $N_2$ fixation from soybean nodules were Peaked at 38 days after planting, and declined thereafter. 3. When calculated upon the basis of the amounts of $N_2$ fixed as measured by acetylene reducing activities in single soybean plant, it was found that the average amount of symbiotic $N_2$ fixation falls in the range of 80 kg N per ha.
For developing the site-specific fertilizer management strategies of crop, it is essential to know the spatial variability of soil factors and to assess their influence on the variability of crop growth and yield. In 2002 and 2003 cropping seasons within-field spatial variability of rice growth and yield was examined in relation to spatial variation of soil properties in the· two paddy fields having each area of ca. $6,600m^2$ in Suwon, Korea. The fields were managed without fertilizer or with uniform application of N, P, and K fertilizer under direct-seeded and transplanted rice. Stable soil properties such as content of clay (Clay), total nitrogen (TN), organic mater (OM), silica (Si), cation exchange capacity (CEC), and rice growth and yield were measured in each grid of $10\times10m$. The two fields showed quite similar spatial variation in soil properties, showing the smallest coefficient of variation (CV) in Clay $(7.6\%)$ and the largest in Si $(21.4\%)$. The CV of plant growth parameters measured at panicle initiation (PIS) and heading stage (HD) ranged from 6 to $38\%$, and that of rice yield ranged from 11 to $21\%$. CEC, OM, TN, and available Si showed significant correlations with rice growth and yield. Multiple linear regression model with stepwise procedure selected independent variables of N fertilizer level, climate condition and soil properties, explaining as much as $76\%$ of yield variability, of which $21.6\%$ is ascribed to soil properties. Among the soil properties, the most important soil factors causing yield spatial variability was OM, followed by Si, TN, and CEC. Boundary line response of rice yield to soil properties was represented well by Mitcherich equation (negative exponential equation) that was used to quantify the influence of soil properties on rice yield, and then the Law of the Minimum was used to identify the soil limiting factor for each grid. This boundary line approach using five stable soil properties as limiting factor explained an average of about $50\%$ of the spatial yield variability. Although the determination coefficient was not very high, an advantage of the method was that it identified clearly which soil parameter was yield limiting factor and where it was distributed in the field.
The three analysis methods, EPA method 3050, the method offered by Ministry of Environment in Korea, and modified method corrected in this laboratory, were studied to investigate the effect of matrix on the analysis of inorganic priority pollutants. 7 inorganic priority pollutants(Ni, Cr, Cu, Zn, Pb, Cd, Hg) were spiked to the plating, leather, paper, electric, and dye sludges. Mean recovery of the elements except Hg was 95.5% when the procedure of EPA method was applied. However, recovery by the two other extraction methods showed 11.1% and 27.7%, respectively. Digestions were done by MDS (microwave digestion system) and $HNO_3+HClO_4$ methods. To study organic and inorganic matrix effect, samples were made by adding triethanol amine as a organic matrix and $FeCl_3{\cdot}6H_2O$+$AlCl_3{\cdot}6H_2O$ as a inorganic matrix, respectively. The extracts were analyzed by AAS and HG-AAS. Mean recovery of the elements by the $HNO_3+HClO_4$ procedure, except Hg, gave better result than that of the MDS method. Mean recovery of elements was decreased when organic and inorganic matrices were added in the sludge samples. The procedure of MDS and $HNO_3+HClO_4$ digestion gave higher recoveries than that of direct analysis. In general, the results of the studies showed a significant matrix effect on the inorganic priority pollutants analysis in sludges.
Voltammetric behavior of some light lanthanide ions($La^{3+}$, $Pr^{3+}$, $Nd^{3+}$, $Sm^{3+}$ and $Eu^{3+}$) in acetonitrile(AN) and dimethylformamide(DMF) has been investigated by direct current, differential pulse polarography and cyclic voltammetry. The reduction of $La^{3+}$, $Pr^{3+}$ and $Nd^{3+}$ in 0.1M TEAP proceeded directly to the metallic state through three-electron charge transfer of irreversible process where as $Sm^{3+}$ and $Eu^{3+}$ proceeded by charge transfer of two steps. As the results of the cyclic voltammetric investigation, the first step reduction of $Sm^{3+}$ and $Eu^{3+}$ were a quasireversible reaction, the second step reductions were an irreversible reaction. The cathodic peak currents of the differential pulse polarogram showed adsorptive properties at lower sweep rates and high concentrations of these metal ions. The peak potenital was shifted to a negative petential and the peak current decreased with the increase of percentage of water in AN. On the other hand, the peak potential was shifted to a positive potential and the peak current decreased with an increased percentage of water in DMF.
Methamphetamine is an amine-containing illegal drug and is distributed unlawfully in South Korea. Finding a rapid, convenient and semi-quantitative determination method for methamphetamine is a very important issue in the area of forensic drug testing. As an effort to develop new screening method, the reactions between three organic compounds which are structurally similar to methamphetamine and N-(9-fluorenylmethoxycarbonyloxy) succinimide (FMOC-NHS) were performed on silica gel ($SiO_2$) TLC plates. Three reference compounds were synthesized and used for the identification, comparison and study of the limit of detection (LOD) of the products obtained from a direct reaction on a TLC plate. As a result, FMOC-NHS as a derivatization reagent generated compounds containing highly UV-active functional groups on the TLC plate after reacting with primary- and secondary amines. In the experiment 2D the LOD of amines was in the range of 0.045 and 0.01 mg/mL ($2{\mu}L/spot$), and in 1D the LOD was in the range of 0.002 and 0.007 mg/mL ($2{\mu}L/spot$). The LODs of the compounds tested were dependent on the concentration of the derivatizing reagent.
A highly purified $(Na^+,\;K^+)-ATPase$ from the rectal gland of Squalus acanthias and from the electric organ of Electrophorus electricus has been used to raise antibodies in rabbits. The 97,000 dalton catalytic subunit and glycoprotein derived from the rectal gland of spiny shark were also used as antigens. The two $(Na^+,\;K^+)-ATPase$ holoenzymes and the two shark subunits were antigenic. In Ouchterlony double diffusion experiments, these antibodies formed precipitation bands with their antigens. Antibodies prepared against the two subunits of shark holoenzyme also formed precipitation bands with their antigens and shark holoenzyme, but not with eel holoenzyme. These observations are in good agreement with inhibitory effect of these antibodies on the catalytic activity of $(Na^+,\;K^+)-ATPase$ both from the shark and the eel, since there is very little cross-reaction between the shark anticatalytic subunit antibodies and the eel holoenzyme. The maximum antibodies titer of the anticatalytic subunit antibodies is found to be 6 weeks after the initial single exposure to this antigen. Multiple injections of the antigen increased the antibody titer. However, the time required to produce the maximum antibody titer was approximately the same. These antibodies also inhibit catalytic activity of $(Na^+,\;K^+)-ATPase$ vesicles reconstituted by a slow dialysis of cholate after solubilization of the enzyme in a presonicated mixture of cholate and phospholipid. In these reconstituted $(Na^+,\;K^+)-ATPase$ vesicles, effects of these antibodies on the fluxes of $Na^+$, $Rb^+$, and $K^+$ were investigated. Control or preimmune serum had no effect on the influx of $^{22}Na^+$ or the efflux of $^{86}Rb^+$. Immunized sera against the shark $(Na^+,\;K^+)-ATPase$ holoenzyme, its glycoprotein or catalytic subunit did inhibit the influx of $^{22}Na^+$ and the efflux of $^{86}Rb^+$. It was also demonstrated that these antibodies inhibit the coupled counter-transport of $Na^+$ and $K^+$ as studied by means of dual labeling experiments. However, this inhibitory effect of the antibodies on transport of ions in the $(Na^+,\;K^+)-ATPase$ vesicles is manifested only on the portion of energy and temperature dependent alkali metal fluxes, not on the portion of ATP and ouabain insensitive ion movement. Simultaneous determination of effects of the antibodies on ion fluxes and vesicular catalytic activity indicates that an inhibition of active ion transport in reconstituted $(Na^+,\;K^+)-ATPase$ vesicles appears to be due to the inhibitory action of the antibodies on the enzymatic activity of $(Na^+,\;K^+)-ATPase$ molecules incorporated in the vesicles. These findings that the inhibitory effects of the antibodies specific to $(Na^+,\;K^+)-ATPase$ or to its subunits on ATP and temperature sensitive monovalent cation transport in parallel with the inhibitory effect of vesicular catalytic activity by these antibodies provide direct evidence that $(Na^+,\;K^+)-ATPase$ is the molecular machinery of active cation transport in this reconstituted $(Na^+,\;K^+)-ATPase$ vesicular system.
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