• Analytical Science and Technology
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• v.24 no.2
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• pp.69-77
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• 2011

Ethylene glycol (EG) is produced commercially in large amounts and is widely used as antifreeze or deicing solution for cars, boats, and aircraft. EG poisoning occurs in suicide attempts and infrequently, either intentionally through misuse or accidental as EG has a sweet taste. EG has in itself a low toxicity, but is in vivo broken down to higher toxic organic acids which are responsible for extensive cellular damage in various tissues caused principally by the metabolites glycolic acid and oxalic acid. The most conclusive analytical method of diagnosing EG poisoning is determination of EG concentration. However, victims are sometimes admitted at a late stage to hospitals or died during emergency treatment like a gastric lavage or found rotten dead, when blood EG concentrations are low or not detected. Therefore, in this study, the identification of EG was not only performed by gas chromatograpyc-mass spectrometry (GC-MS) following derivatization but also further toxicological analyses of metabolites, glycolic acid (GA) and oxalic acid (OA), were performed by ion chromatography in various biological specimens. A ranges of blood concentrations (3 cases) was $10\sim2,400\;{\mu}g/mL$ for EG, $224\sim1,164\;{\mu}g/mL$ for GA and ND $\sim40\;{\mu}g/mL$ for OA, respectively, In other biological specimens (liver, kidney, bile and pleural fluid), a range of concentrations (3 cases) was ND $\sim55,000\;{\mu}g/mL$ for EG, ND $\sim1,124\;{\mu}g/mL$ for GA and ND $\sim60\;{\mu}g/mL$ for OA, respectively. Liver and kidney tissues were recommended specimens including blood because OA, a final metabolite of EG, was identified large amounts in these despite no detectable EG caused by some therapy.

• Journal of Korean Society for Atmospheric Environment
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• v.15 no.2
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• pp.89-100
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• 1999

The rain water samples were collected at Chunchon and Seoul by using wet only automatic sampler from January 1996 through 1997. The daily base rain water samples collected over than 95% rainy events components, $SO_4^{-2}$, $NO_3^-$, $CI^-$, NH_4^+$, $Ca^{2+}$, $Mg^{2+}$, $Na^+$, and $K^+$, by ion chromatography. In 1996, about 77% of sampled rain water showed below pH 5.6 and the 60% of rain water was lower than pH 5.0. The volume weighted average pH was 4.7 at all sites. In 1997, the volume weighted average pH was 4.6 and 4.9 at Seoul and Chunchon, respectively. Among the rain water samples,, 87% and 55% fo samples showed below than pH 5.6 and 5.0, respectively. The pH value of Chunchon was significantly (p＜0.05) lower than Seoul at the rain samples for less than 20mm rainfall. However conductivity of the rain samples were 20.9$\mu$S/cm for 1996 and 27.7$\mu$S/cm for 1997 at Seoul, and 19.1$\mu$S/cm for 1996 and 14.1$\mu$S/cm for 1997 at Chunchon. $H_2SO_4$ and $HNO_3$ contributed 65.9% and 29.6% of free acidity at Seoul, respectively. The ratio of [$NO_3^-$]/[nss-$SO_4^{-2}$] were 0.43 at Seoul and 0.51 at Chunchon for rain samples for less than 20mm rainfall. The annual wet deposition of $CI^-$, $NO_3^-$, $SO_4^{-2}$, $H^+$M, $Na^+$, NH_4^+$, $K^+$, $Mg^{2+}$, and $Ca^{2+}$, respectively, 568.8kg/$ extrm{km}^2$, 1489.3kg/$\textrm{km}^2$, 3184.8kg/$\textrm{km}^2$, 20.9kg/$\textrm{km}^2$, 249.4kg/$\textrm{km}^2$, 1091.2kg/$\textrm{km}^2$, 189.8kg/ $\textrm{km}^2$, 90.2kg/$\textrm{km}^2$ and 702.4kg/$\textrm{km}^2$ at Seoul for 1996; 656.4kg/$\textrm{km}^2$, 2029.7kg/$\textrm{km}^2$, 3280.7kg/$\textrm{km}^2$, 27.2kg /$\textrm{km}^2$, 229.4kg/$\textrm{km}^2$, 1063.9kg/$\textrm{km}^2$, 106.9kg/$\textrm{km}^2$, 78.2kg/$\textrm{km}^2$, 645.3kg/$\textrm{km}^2$ at Seoul for 1997; 116.9kg/ $\textrm{km}^2$, 983.3kg/$\textrm{km}^2$, 1797.0kg/$\textrm{km}^2$, 21.4kg/$\textrm{km}^2$, 83.2kg/$\textrm{km}^2$, 648.1kg/$\textrm{km}^2$, 78.0kg/$\textrm{km}^2$, 22.2kg/$\textrm{km}^2$, 368.8kg/$\textrm{km}^2$ at chunchon for 1996; 100.2kg/$\textrm{km}^2$, 1077.6kg/$\textrm{km}^2$, 1754.0kg/$\textrm{km}^2$, 13.4kg/$\textrm{km}^2$, 146.0kg/$\textrm{km}^2$, 602.3kg/$\textrm{km}^2$, 88.8kg/$\textrm{km}^2$, 16.2kg/$\textrm{km}^2$ and 206.8kg/$\textrm{km}^2$ at chunchon for 1997.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.4 no.1
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• pp.31-41
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• 1971

The present study was directed to define the degradation pattern of the nucleotides and their related compounds in the muscle of anchovy during drying. Three kinds of samples, fresh, sun dried and boiled-and-dried anchovy, were prepared and the contents of nucleotides and related compounds of samples were determined by ion exchange chromatography. The results obtained are summarized as follows: Almost all of ATP disappeared in both muscle of sun dried and boiled-and-dried anchovy, although the initial content of ATP in fresh muscle was very low ($1.8{\mu}moles/g$, dry basis). But the remainning amount of ADP was considerably high while the other nucleotide almost entirely disappeared. This suggested that the residual ADP is responsible to the 'bound nucleotide' of myofibrils. In general, AMP content was comparatively lower than that of other nucleotides. Among three samples, the boiled-and-dried sample showed relatively higher AMP value than others. The amount of IMP remained in muscle remarkably varied between the boiled-and-dried anchovy and sun dried anchovy, the former's value being sixteen times higher than that of latter. In the contents of inosine and hypoxanthine, the sun dried anchovy marked an exceedingly high value equivalent to 2.7 times of the boiled-and-dried anchovy. In comparison of the ratio of inosine and hypoxanthine, hypoxanthine was accumulating in boiled-and-dried anchovy whereas inosine was in the sun-dried anchovy. Eighty three percent of total nucleotides in the fresh anchovy retained in the boiled-and-dried anchovy and IMP ratio in total nucleotides was $73\%$. On the contrary, the sun dried anchovy showed barely $10\%$ of retention rate and IMP ratio was only $38\%$. Considered from the flavor quality of dried anchovy, so far as concerned IMP content, it may be said that the boiled-and-drying method is more favorable process for dried product of anchovy than the sun-drying method.

• Journal of Life Science
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• v.19 no.9
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• pp.1218-1225
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• 2009

Difractose anhydrides (DFAs) is studied as a sweetener for diabetics because of its structural property. DFAs have four types: DFA I, III, IV (degradation of levan) and V (degradation of inulin). Especially, DFA IV has been shown to enhance the absorption of calcium in experiments using rats. Levan fructotransferase is an enzyme for producing di-d-fructose-2,6':6,2-dianhydride (DFA IV). To identify structural characterization, we purified wild-type and mutants (D63A, D195N and N85S) of levan fructotransferase (LFTase) from Microbacterium sp. AL-210. These proteins were purified to apparent homogeneity by Ni-NTA affinity column, Q-sepharose ion exchange and gel filtration chromatography and detected by SDS-PAGE. They were also analyzed by circular dichroism (CD) measurements, JNET secondary structure prediction, activity measurements at various temperatures, and pH analysis. The optimum pH for the enzyme-catalyzed reaction was pH 7.5 and optimum temperature was observed at $55^{\circ}C$. Along with wild-type LFTase, mutants were analyzed by CD measurement, fluorescence analysis and differential scanning calorimetry (DSC). N85S showed less $\alpha$-helix and more $\beta$ strand than others. Also, N85S showed almost the same curve as wild-type in their steady-state fluorescence spectra, whereas mutant D63A and D195N showed higher intensity than wild-type. The amino acid sequence of wild-type LFTase was compared to the sequences of exo-inulinase from Aspergillus awamori, a plant fructan 1-exohydrolase from Cichorium intybus, and Thermotogo maritime (Tm) invertase and showed a high identity with Exo-inulinase from Aspergillus awamori.

• Journal of Korean Society of Environmental Engineers
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• v.30 no.3
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• pp.302-313
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• 2008

The purposes of this study are to investigate the concentration levels of fine particles, so called PM$_{2.5}$, to identify the affecting sources, and to estimate quantitatively the source contributions of PM$_{2.5}$. Ambient air sampling was seasonally carried out at two sites in Pohang(a residential and an industrial area) during the period of March to December 2003. PM$_{2.5}$ samples were collected by high volume air samplers with a PM$_{10}$ Inlet and an impactor for particle size segregation, and then determined by gravimetric method. The chemical species associated with PM$_{2.5}$ were analyzed by inductively coupled plasma spectrophotometery(ICP) and ion chromatography(IC). The results showed that the most significant season for PM$_{2.5}$ mass concentrations appeared to be spring, followed by winter, fall, and summer. The annual mean concentrations of PM$_{2.5}$ were 36.6 $\mu$g/m$^3$ in the industrial and 30.6 $\mu$g/m$^3$ in the residential area, respectively. The major components associated with PM$_{2.5}$ were the secondary aerosols such as nitrates and sulfates, which were respectively 4.2 and 8.6 $\mu$g/m$^3$ in the industrial area and 3.7 and 6.9 $\mu$g/m$^3$ in the residential area. The concentrations of chemical component in relation to natural emission sources such as Al, Ca, Mg, K were generally higher at both sampling sites than other sources. However, the concentrations of Fe, Mn, Cr in the industrial area were higher than those in the residential area. Based on the principal component analysis and stepwise multiple linear regression analysis for both areas, it was found that soil/road dust and secondary aerosols are the most significant factors affecting the variations of PM$_{2.5}$ in the ambient air of Pohang. The source apportionments of PM$_{2.5}$ were conducted by chemical mass balance(CMB) modeling. The contributions of PM$_{2.5}$ emission sources were estimated using the CMB8.0 receptor model, resulting that soil/road dust was the major contributor to PM$_{2.5}$, followed by secondary aerosols, vehicle emissions, marine aerosols, metallurgy industry. Finally, the application and its limitations of chemical mass balance modeling for PM$_{2.5}$ was discussed.

• The Korean Journal of Pesticide Science
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• v.15 no.3
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• pp.254-268
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• 2011

Fenoxycarb, pyriproxyfen and methoprene are juvenile hormone mimic insecticide. These insecticides have been widely used for mosquito, fly, scale insects, and Lepidoptera. The purpose of this study was to develop a simultaneous determination procedure of fenoxycarb, pyriproxyfen and methoprene residues in crops using HPLC-UVD/MS. These insecticide residues were extracted with acetone from representative samples of four raw products which comprised brown rice, apple, green pepper, and Chinese cabbage. The extract was diluted with saline water, and then n-hexane/dichloromethane partition was followed to recover these insecticides from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The analytes were quantitated by HPLC-UVD/MS, using a $C_{18}$ column. The crops were fortified with each insecticide at 3 levels per crop. Mean recovery ratios were ranged from 80.0 to 104.3% in four representative agricultural commodities. The coefficients of variation were less than 4.8%. Quantitative limit of fenoxycarb, pyriproxyfen, and methoprene was 0.04 mg/kg in crop samples. A HPLC-UVD/MS with selected-ion monitoring was also provided to confirm the suspected residues. The proposed simultaneous analysis method was reproducible and sensitive enough to determine the residues of fenoxycarb, pyriproxyfen and methoprene in the agricultural commodities.

• Korean Journal of Food Science and Technology
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• v.39 no.4
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• pp.372-379
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• 2007

A high-performance liquid chromatography-electrospray ionization (HPLC-ESI) tandem MS was developed for the rapid and simultaneous determination of forbidden medicines in dietary supplements. Thirteen medicinal components such as PDE-5 inhibitors and their analogues, and the newly identified dimethylsildenafil and xanthoanthrafil, were included in this study. After tentative standardization of molecular ions in both polarities using thirteen references on the mass spectrometer, with ESI-continuous infusion via the syringe pump method, the relative intensity of the ions present in the resulting spectra was quantitatively compared. From the results, the ion mode was selected depending on each reference's characteristics. A HPLC method coupled with the ESI mode was developed considering the matrix effect and interference depending on the type of sample. The validation test of the developed method was followed by carrying out precision, accuracy, recovery, sensitivity and linearity, etc. The method showed sufficiently high sensitivity, reproducibility, and specificity, and produced 4 times faster results when compared with the existing HPLC/UV method for the determination of forbidden compounds in dietary supplements.

• Applied Biological Chemistry
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• v.15 no.2
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• pp.111-142
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• 1972

An experimental Chung-Kook-Jang was prepared using the strain Bacillus subtilis sp. isolated by the author Samples were taken in 12 hrs interval during the fermentation and the oligopeptides were separated by the method of molecular sieving using the ion exchange resin column of Dowex-50. Only the X-16 fraction of oligopeptides was taken and the components of oligopeptides were developed in two dimensional thin layer chromatograms. The each peptide spot was eluted and each peptide was isolated. The pattern and kinds of amino acids, and N and C-terminal amino acids were studied. Fourteen different oligopeptides could be detected by the two dimensional thin layer chromatography, all of which were consisted of $4{\sim}9$ kinds of amino acids. No dipeptides and no tripeptides could be found. The N and C-terminal amino acids and the residual component amino acids of all these 14 peptides could be summarized as the follows. [P]-I. Pro (Cys Ala Asp Trp Ile Val) Glu [P]-II. Val (His Arg Glu Thr Ala Met) Asp [P]-III. Glu (Cys Lys Asp Thr Met) Ala [P]-IV. Glu(His Ser Ala) Met) [P]-V. Ile (Cys Asp Arg Gly Pro T.p Phe) His [P]-VI. Gly(Asp ser) Lys [P]-VII. Thr(Pro Tyr Phe) Asp [P]-VIII. Phe(Tyr Leu Ile) Val [P]-IX. Trp (Phelle) Thr [P]-X. Ile (Arg Leu) Phe [P]-XI. Asp (Lys His Ser Gly Glu Pro) Ala [P]-XII. Glu (Cys Asp Gly) Ser [P]-XIII. Ala (Arg Tyr) Glu [P]-XIV. Met (Glu Ala) His It appears that the protease of the Bacillus subtilis K-27 syrain has rather wider range of specificity than proteases of Aspergoillus soya, pepsin, chymotrypsin, and trypsin.

• Korean Journal of Environmental Agriculture
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• v.31 no.2
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• pp.157-163
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• 2012

BACKGROUND: For the safety of imported agricultural products, the study was conducted to develop the analytical method of unregistered pesticides in domestic. The analytical method of 6 pesticides, chlorthal-dimethyl, clomeprop, diflufenican, hexachlorobenzene, picolinafen, and propyzamide, for a fast multi-residue analysis were established for two different type crops, orange and brown rice by GC-ECD and confirmed by mass spectrometry. METHODS AND RESULTS: The analytical method was evaluated to limit of quantification, linearity and recoveries. The crop samples were extracted with acetonitrile and performed cleanup by liquid-liquid partition and Florisil SPE to remove co-extracted matrix. The extracted samples were analyzed by GC-ECD with good sensitivity and selectivity of the method. The limits of quantification (LOQ) range of the method with S/N ratio of 10 was 0.02~0.05 mg/kg for orange and brown rice. The linearity for targeted pesticides were $R^2$ >0.999 at the levels ranged from 0.05 to 10.0 mg/kg. The average recoveries ranged from 74.4% to 110.3% with the percentage of coefficient variation in the range 0.2~8.8% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in brown rice. And the average recoveries ranged from 77.8% to 118.4% with the percentage of coefficient variation in the range 0.2~6.6% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in orange. Final determination was by gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) to identify the targeted pesticides. CONCLUSION: As a result, this developed analytical method can be used as an official method for imported agricultural products.

• Analytical Science and Technology
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• v.23 no.2
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• pp.187-195
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• 2010

To assess health risk for the intake among residents after the Hebei Spirit oil spill, 16 Polycyclic Aromatic Hydrocarbons (PAHs) in seafood samples from oil contaminated bay were determined by Gas Chromatography-Mass Spectrometry (GC-MSD) and samples were personally collected and purchased by residents. Samples were hydrolyzed with KOH and extracted with methylene chloride. The extracted solution were cleaned up using silica/florisil column and 16 PAHs were eluted by methylene chloride : n-hexane (1:9) mixture and determined by GC-MSD in Selected Ion Monitoring (SIM) mode. The mean recoveries for 16 PAHs ranged from 79% to 85%. The 16 PAHs levels in 126 samples ranged from 0.17 to $6.04\;{\mu}g$/kg and the TEQBaP (Toxic EQuivalents) levels in 126 samples were calculated using benzo(a)pyrene toxic equivalency factor for individual 16 PAHs and ranged from 0 to $0.91\;{\mu}gTEQ$/kg. The average Benzo(a)pyrene dietary exposure of residents was $5.5{\times}10^{-8}\;mg/kg$ bw/day and the average PAHs chronic dietary exposure was $1.3{\times}10^{-5}\;mg$ TEQ/kg bw/day. The margin of exposure (MOE) and the excess cancer risk and were $1.8{\times}10^6$ and $9.8{\times}10^{-8}$, respectively. Therefore, the assessment result was considered as low concern for health risk.