• The Korean Journal of Pesticide Science
• /
• v.21 no.1
• /
• pp.75-83
• /
• 2017

The single residue analytical method was developed for determining fungicide pencycuron residues in various agricultural commodities with high-performance liquid chromatography (HPLC). Pencycuron residue was extracted with acetone from representative crops such as Korean cabbage, apple, brown rice and green pepper. After ethyl acetate/n-hexane partition and subsequent clean-up with silica gel chromatography, pencycuron residue was quantified by reversed phase HPLC with UV detection at 240 nm. The suspected residue of pencycuron was confirmed using selected-ion monitoring (SIM) LC/mass spectrometry (MS). Instrumental limit of quantitation (ILOQ) and method LOQ (MLOQ) were set at 2 ng and 0.02 mg/kg, respectively. Overall recoveries of pencycuron from different crop samples fortified at three levels (MLOQ, 10MLOQ, 100MLOQ) were 72~108%. This proposed method could be useful as official analytical method for quantification of pencycuron residues in agricultural commodities.

• Journal of Astronomy and Space Sciences
• /
• v.26 no.4
• /
• pp.567-588
• /
• 2009

Korea-Japan Joint VLBI Correlator (KJJVC) is being developed by collaborating KASI (Korea Astronomy and Space Science Institute), Korea, and NAOJ(National Observatory of Japan), Japan. In early 2010, KJJVC will work in normal operation. In this study, we developed the software correlator which is based on VCS (VLBI Correlation Subsystem) hardware specification as the core component of KJJVC. The main specification of software correlator is 8 Gbps, 8192 output channels, and 262,144-points FFT (Fast Fourier Transform) function same as VCS. And the functional algorithm which is same as specification of VCS and arithmetic register are adopted in this software correlator. To verify the performance of developed software correlator, the correlation experiments were carried out using the spectral line and continuum sources which were observed by VERA (VLBI Exploration of Radio Astrometry), NAOJ. And the experimental results were compared to the output of Mitaka FX correlator by referring spectrum shape, phase rate, and fringe detection and so on. Through the experimental results, we confirmed that the correlation results of software correlator are the same as Mitaka FX correlator and verified the effectiveness of it. In future, we expect that the developed software correlator will be the possible software correlator of KVN (Korean VLBI Network) with KJJVC by introducing the correlation post-processing and modifying the user interface as like GUI (Graphic User Interface).

• Journal of Korean Neurosurgical Society
• /
• v.37 no.6
• /
• pp.443-448
• /
• 2005

Objective: A variety of genetic alterations in human glioblastoma comprises signal transduction and cell cycle arrest control of cellular processes. Subtractive hybridization is potentially a faster method for identifying differentially expressed genes associated with a particular disease state. Using the technique of subtraction, we isolated novel genes that are overexpressed in glioblastoma tissue as compared to normal brain tissue. Methods: We evaluated the differential expression of genes in each of hybridizing tester and driver cDNAs to digested 130 clones. After sequencing of 130 clones and homology search, this study performed to determine mRNA expression of the unknown gene, "clone 47", in brain tissue, glioblasoma, and several cancer cell lines by reverse transcription-polymerase chain reaction (RT-PCR). To test the time course for Go-phase arrest, serum stimulation and expression at various times for RT-PCR performed. Results: We identified 23 novel genes by BLAST of the digested 130 clones. The expressions of "clone 47" mRNA of glioblastoma and several cancer lines were significantly higher than normal brain tissues and several normal cell lines. We confirmed the mRNA expression of "clone 47" was up-regulation for $0.5{\sim}1hr$ of WI-38 cell differentiation. Conclusion: The novel gene, "Clone 47" is upregulated in glioblastoma tissue and several cancer cell lines. This gene is time dependent activation during time course of serum stimulation. This result suggests that "clone 47" playa role in brain tumorigenesis and the activation of this "clone 47" may be necessary for the development of cancer.

• Journal of the Society of Cosmetic Scientists of Korea
• /
• v.42 no.1
• /
• pp.65-73
• /
• 2016

Korea Food and Drug Administration (KFDA) has officially announced 2,4-dinitrophenylhydrazine (DNPH) derivatization - high performance liquid chromatography (HPLC) methods for analysis of formaldehyde. This study was conducted to develop a convenient derivatization method for cosmetics by improving complex pre-treatment procedures included in KFDA method. To simplify pre-treatment procedures of KFDA method, reaction conditions including pH, time and temperature were optimized. This pre-treatment method does not require complicate pre-treatment steps of KFDA method such as pH adjustment of test solution with acetate buffer (pH 5.0), solvent-solvent partitioning with dichloromethane and concentrating procedure with vacuum evaporator. Formaldehyde-dinitrophenylhydrazone (formaldehyde-DNP) product produced by derivatization reaction was separated and quantified with a reversed-phase HPLC, which was slightly modified with KFDA method. The linearity test showed good results with 0.9999 of correlation coefficient ($r^2$) in the range of 2 ~ 40 ppm of standard solutions. In this method, limit of detection (LOD) and limit of quantitation (LOQ) values for formaldehyde were 0.2 ppm and 0.5 ppm, respectively. In addition, recovery test demonstrated that the method was also accurate and reproducible. Therefore, the proposed method can be applicable to rapid analysis of formaldehyde in cosmetics.

• Journal of the Korean Wood Science and Technology
• /
• v.44 no.3
• /
• pp.337-349
• /
• 2016

In this study, an analytical method to evaluate the quality of isoflavonoid compounds purified and isolated from the fruits of Cudrania tricuspidata was developed and validated using Ultra Performance Liquid Chromatography (UPLC). The fruits of C. tricuspidata were extracted with methanol and further fractioned with n-hexane, ethyl acetate and water. The resulting ethyl acetate extract separated into four isoflavonoid compounds by a combination of silica gel and sephadex LH-20 column chromatography. The structures of the compounds were elucidated as alpinumisoflavone, 6,8-diprenyl genistein, 6,8-diprenyl orobol, 4'-O-methylalpinumisoflavone by various techniques such as UV-Vis, ESI-MS, $^1H\;NMR$ and $^{13}C\;NMR$ spectroscopy. Finally, a method to characterize the compounds was developed by using the UPLC equipped with a $C_{18}$ column and a gradient mobile phase system consisting of 2% acetic acid in water (solvent A) and 2% acetic acid in methanol (solvent B). The developed method was validated with the parameters such as selectivity, linearity, limit of detection, limit of quantitation, accuracy, and precision, which are defined by the ICH (International Conference on Harmonization). Using the validated method, the compounds in the fruits harvested in different months were also quantitatively analyzed. We propose this approach this approach can readily be utilized as an efficient evaluation method to quantify the extracts of C. tricuspidata.

• Journal of Environmental Health Sciences
• /
• v.40 no.2
• /
• pp.114-126
• /
• 2014

Objectives: We aimed to develop a measurement method of five metabolites of trichloroethylene (TCE) in a concurrent biological sample, e.g., trichloroacetic acid (TCA), dichloroacetic acid (DCA), S-(1,2-dichlorovinyl) glutathione (DCVG), S-(1,2-dichlorovinyl)-L-cysteine (DCVC), and N-Acetyl-S-(1,2-dichlorovinyl)-L-cysteine (NAcDCVC) and to validate the method before application to pharmacokinetic study. Methods: TCE metabolites were simultaneously analyzed using high performance liquid chromatography coupled with electrospray ionization mass spectrometry (HPLC-ESI-MS/MS) with as little as 50 ${\mu}L$ of serum and urine. DCA, TCA and NAcDCVC were extracted with diethyl ether, while DCVC and DCVG were extracted by solid phase extraction. This method was validated according to the guidelines for bioanalytical method validation of the Korean National Institute of Toxicological Research. Then, we determined the five metabolites in five strains of mice at 24 hr after exposure to 1 g TCE /kg body weight. Results: The limits of detection for the five metabolites in biological samples ranged from 0.001 to 0.076 nmol/mL, which is comparable to or better than those previously reported. Most calibration curves showed good linearity ($R^2=0.99$), and between-batch variation was less than 20% expressing acceptable robustness and reproducibility. Using this method, we found TCA and DCA were detected in all test mice at 24 hr after the oral administration while NAcDCVC and DCVC were detected in some strains, which showed strain-dependent metabolism of TCE. Conclusions: The present method could provide robust and accurate measurements of major key metabolites of TCE in biological media, which allowed concurrent analysis of TCE metabolism for limited amounts of biospecimens.

• Journal of the Korean Society of Food Science and Nutrition
• /
• v.45 no.7
• /
• pp.990-995
• /
• 2016

In the present study, reversed-phase HPLC was utilized to quantify the ${\beta}$-carotene content of 22 kinds of raw and blanched vegetables consumed in Korea. In addition, true retention (TR) of ${\beta}$-carotene in samples was obtained. For quantification of ${\beta}$-carotene, external standard curve was obtained with limit of detection and limit of quantitation. The ${\beta}$-carotene contents in 22 raw vegetables ranged from 6.29 (bellflower root) to $7,050.73{\mu}g/100g$ (spinach, field culture). After blanching, ${\beta}$-carotene contents of 13 vegetables increased up to 103.05% while nine vegetables resulted in reduced content, ranging from -2.17 to -29.16%. However, even though increased ${\beta}$-carotene content was observed after blanching, TR of some vegetables was lower than 100% due to their weight reduction. The highest TR of ${\beta}$-carotene was found from blanched cabbage (164.46%) while the lowest TR was found from Turcz (Gomchwi) at 59.35%. TR is an effective method to evaluate retention of nutrients in cooked foods, considering changes of nutrient content and weight.

• Journal of fish pathology
• /
• v.19 no.2
• /
• pp.155-164
• /
• 2006

Tissue distribution and residue depletion of oxytetracycline (OTC) and tetracycline (TC) following dipping administration were evaluated in olive flounder (Paralichthys olivaceus), rockfish (Sebastes schlegeli), and red sea bream (Pagrus major) under field conditions. Fishes were held in floating cages placed in sea water and fed a commercial diet for 15 days to acclimate to a new surrounding. Fishes were dipped in OTC 50 g/ton water for 30min and TC 18 g/ton water for 5 hours. Blood and muscle were sampled from fishes on 0th, 1th, 2th, 3th, and 5th day after administration. After solid-phase extraction, OTC and TC analyses were carried out by HPLC. The recovery rate of OTC in serum and muscle samples was 71-77% and 78-84%, respectively. Also, the recovery rate of TC in serum and muscle samples was 70-79% and 73-78%, respectively. The results of recovery rate were similar to previous studies reported. At the termination of dipping administration of OTC and TC, residue concentration in muscle samples of rockfish was significantly higher than those of olive flounder and red sea bream. At day 5, residue concentrations of all samples were believed to decrease to lower than 0.05 mg/kg, the detection limit. The present study showed that residue concentrations of OTC and TC decreased to below 0.05 mg/kg after treatment 5th day, faster than the established withdrawal period. The tissue reside depletion time of dipping administration of OTC and TC seems to be shorter than those of oral or parenteral administration.

• Journal of the Korean Society of Food Science and Nutrition
• /
• v.39 no.8
• /
• pp.1231-1235
• /
• 2010

The method for residue analysis of four sulfonylurea pesticides, rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl and chlorimuron-ethyl was examined and analyzed by HPLC with ODS column ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$ diameter particle size) which was maintained at $35^{\circ}C$. Mobile phase consisted of solvent A (20 mM $KH_2PO_4$, pH 2.5) and solvent B (acetonitrile). Isocratic elution of the column with 45% solvent A and 55% solvent B at a flow rate of 1 mL/min resulted in retention times of 5.92, 6.54, 9.28, and 14.35 min for rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl, and chlorimuron-ethyl, respectively. All injection volumes were $20\;{\mu}L$. The limit of quantitation was 0.02, 0.01, 0.001, and 0.004 mg/kg for rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl, and chlorimuron-ethyl, respectively. Recovery rate test was performed with three farm products, rice, apple and soybean. Four sulfonylurea pesticides were spiked at concentrations of 0.05, 0.1 and 0.5 mg/kg. The recovery rates were ranged from 86.12% to 116.26% and the standard deviations of all experiments were within 10%.

• Asian-Australasian Journal of Animal Sciences
• /
• v.33 no.1
• /
• pp.100-110
• /
• 2020

Objective: The objective of this study was to isolate proteolytic microorganisms and evaluate their effects on proteolysis in total mixed ration (TMR) silages of soybean curd residue. Methods: TMRs were formulated with soybean curd residue, alfalfa or Leymus chinensis hay, corn meal, soybean meal, a vitamin-mineral supplement, and salt in a ratio of 25.0: 40.0:30.0:4.0:0.5:0.5, respectively, on a basis of dry matter. The microbial proteinases during ensiling were characterized, the dominate strains associated with proteolysis were identified, and their enzymatic characterization were evaluated in alfalfa (A-TMR) and Leymus chinensis (L-TMR) TMR silages containing soybean curd residue. Results: Both A-TMR and L-TMR silages were well preserved, with low pH and high lactic acid concentrations. The aerobic bacteria and yeast counts in both TMR silages decreased to about 10⁵ cfu/g fresh matter (FM) and below the detection limit, respectively. The lactic acid bacteria count increased to 10⁹ cfu/g FM. The total microbial proteinases activities reached their maximums during the early ensiling stage and then reduced in both TMR silages with fermentation prolonged. Metalloproteinase was the main proteinase when the total proteinases activities reached their maximums, and when ensiling terminated, metallo and serine proteinases played equally important parts in proteolysis in both TMR silages. Strains in the genera Curtobacterium and Paenibacillus were identified as the most dominant proteolytic bacteria in A-TMR and L-TMR, respectively, and both their proteinases were mainly with metalloproteinase characteristics. In the latter ensiling phase, Enterococcus faecium strains became the major sources of proteolytic enzymes in both TMR silages. Their proteinases were mainly of metallo and serine proteinases classes in this experiment. Conclusion: Proteolytic aerobic bacteria were substituted by proteolytic lactic acid bacteria during ensiling, and the microbial serine and metallo proteinases in these strains played leading roles in proteolysis in TMR silages.