• 대한화학회지
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• 제27권5호
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• pp.345-352
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• 1983

Diphenylcarbazide를 흡착시킨 큰 그물구조 수지를 사용하여 컬럼 조작에 의해 0.1M 황산수용액에서 크롬(Ⅵ)이온을 선택적으로 농축하였다. 시료수의 액성과 유속을 조절하여 각종 수지에 대해 크롬(Ⅵ)이온 추출실험을 한 결과 Diaion HP-20이 가장 큰 돌파교환용량을 나타내었다. Diaion HP-20에 대해 크롬(Ⅵ)이온의 돌파점은 흡착된 DPC의 농도에 비례하였으며 크롬(Ⅵ)이온의 농도가 진할 때가 묽을 때 보다 높은 돌파교환용량을 나타냈다. 또한 일반 환경수 속에 공존되기 쉬운 각종 중금속 이온들에 대한 크롬(Ⅵ)이온의 농축에 미치는 영향을 조사한 결과 10ppm 크롬(Ⅵ)이온에 대해 철(Ⅲ)이온을 제외한 모든 금속 이온들은 100배까지 공존하여도 영향을 미치지 않았으며 철(Ⅲ)이온은 10배까지 방해되지 않았다. 크롬(Ⅵ)이온 추출에 이용된 겔 입자는 메탄올로서 쉽고도 효과적으로 재생되므로 반복 사용할 수 있다.

• 대한수의학회지
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• 제37권1호
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• pp.195-202
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• 1997

A method for the isolation by matrix solid phase dispersion method and liquid chromatographic determination of enrofloxacin and ciprofloxacin in pork muscle tissue is presented. Blank or enrofloxacin and ciprofloxacin spiked samples(0.5g) containing 0.05g oxalic acid were blended with $C_{18}$(octadecylsilyl derivatized silica) packing material. After homogenization, $C_{18}$/muscle tissue matrix was transferred to glass column made from 10ml glass syringe and filter paper, and compressed to 4~4.5ml volume. A column was washed with 8ml of hexane and dried under vacuum. Interfering materials were removed by ethylacetate 8ml and dried, following which enrofloxacin and ciprofloxacin were eluted with 8ml of methanal under gravity. The eluate containing enrofloxacin and ciprofloxacin wase free from interfering compound when analysed by HPLC with UV detection at 278nm. Enrofloxacin and ciprofloxacin showed linear response with UV detector at the range of $0.05{\sim}1.0{\mu}g/ml$ and eluted within 5ml elution volume of methanol from the matrix. Fortified sample containing 0.05g oxalic acid represented more good recoveries than that of control sample. Average percentages of enrofloxacin and ciprofloxacin were $93.30{\pm}4.56%$ and $91.84{\pm}4.17%$, respectively, for the concentration range(0.05, 0.1, 0.25, 0.5 and $0.75{\mu}g/g$). The interassay variability of enrofloxacin was $6.02{\pm}5.33%$ with an intra-assay variability of 4.89% and $6.75{\pm}2.68%$ with 4.54% for ciprofloxacin. Detection limit of enrofloxacin and ciprofloxacin was $0.030{\mu}g/g$ in the spiked sample.

• Journal of Microbiology and Biotechnology
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• 제23권3호
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• pp.313-321
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• 2013

Bacillus subtilis XF-1, a strain with demonstrated ability to control clubroot disease caused by Plasmodiophora brassicae, was studied to elucidate its mechanism of antifungal activity against P. brassicae. Fengycin-type cyclopeptides (FTCPs), a well-known class of compounds with strong fungitoxic activity, were purified by acid precipitation, methanol extraction, and chromatographic separation. Eight homologs of fengycin, seven homologs of dehydroxyfengycin, and six unknown FTCPs were characterized with LC/ESI-MS, LC/ESI-MS/MS, and NMR. FTCPs (250 ${\mu}g/ml$) were used to treat the resting spores of P. brassicae ($10^7/ml$) by detecting leakage of the cytoplasm components and cell destruction. After 12 h treatment, the absorbencies at 260 nm ($A_{260}$) and at 280 nm ($A_{280}$) increased gradually to approaching the maximum of absorbance, accompanying the collapse of P. brassicae resting spores, and nearly no complete cells were observed at 24 h treatment. The results suggested that the cells could be cleaved by the FTCPs of B. subtilis XF-1, and the diversity of FTCPs was mainly attributed to a mechanism of clubroot disease biocontrol.

• 약학회지
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• 제52권2호
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• pp.93-100
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• 2008

A liquid chromatographic method with tandom spectrometric detection (LC/MS/MS) for the simultaneous determination of doxifluridine and its active metabolite, 5-fluorouracil (5-FU) was developed over the concentration range of $5{\sim}2000$ ng/ml, respectively. Doxifluridine, 5-FU and internal standard, 5-chlorouracil (5-CU), were extracted from liver and intestine tissue via protein precipitation. Acetonitrile was used as the extraction solvent and the supernatant was evaporated and reconstructed in mobile phase. Optimum chromatographic separation was achieved on a Agilent Zorbax $C_{18}$ ($100\;mm{\times}2.1\;mm$, $3.5\;{\mu}m$) column with mobile phase run in isocratic with methanol : water (20 : 80, v/v). The flow rate was 0.2 ml/min with total cycle time of 5 min. The lower limit of quantification was validated at 5.0 ng/ml of liver and intestine tissue, for both doxifluridine and 5-FU, respectively. The intra-day and inter-day precision and accuracy of quality control (QC) samples were <11% coefficient of variation and <7% relative error from theoretical concentration for both analytes. In addition, the special designed stability study was performed, because the metabolism of doxifluridine occurs spontaneously even in ice bath for monkey liver. The stability of doxifluridine in liver and intestine of monkey and beagle dog was compared. It was found that bioanalytical validation could not be performed for the monkey liver; however, beagle dog's liver has relatively low speed of metabolism compared to monkey liver and instead of monkey liver, beagle dog's liver could be used for the validation. Bioanalytical validation could be performed in monkey intestine. Eventually, this developed method for liver and intestine will be useful in support of the toxicokinetic and pharmacokinetic studies of doxifluridine and 5-FU.

• 한국식품조리과학회지
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• 제31권5호
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• pp.581-587
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• 2015

This study was conducted to investigate the antioxidative and antimicrobial activities of Korean dandelion (Taraxacum coreanum). Water extracts, ethanol extracts and methanol extracts were used to examine the free radical scavenging activity, total flavonoid content, total polyphenol content and antimicrobial activity. The free radical scavenging activity, total flavonoid, total polyphenol and total antioxidant activity of the water extracts were higher than those of the other extraction solvents. The antimicrobial activties of Korean dandelion extracts were examined on several food borne illness microorganisms using the paper disc diffusion method. Inhibition zones were observed on Staphylococcus aureus subsp. aureus, Listeria monocytogenes, Bacillus subtilis, Bacillus cereus and Escherichia coli in ethanol extracts. Inhibition zones were also observed on Listeria monocytogenes in water extracts. The physico-chemical properties of Korean dandelion tea according to the roasting time and soaking amount of tea were studied. The pH of the dandelion tea significantly decreased while the soluble solid contents significantly increased with increased roasting time (p<0.01). The lightness of the dandelion tea decreased and the turbidity increased with increased roasting time. In sensory evaluation, the sensory scores for the color, flavor and total acceptability were highest in the 40 min roasted tea. These results suggest that the water extract of Korean dandelion could be used as an antioxidative and antimicrobial functional food source. The optimum roasting time for Korean dandelion tea was 40 min at $200^{\circ}C$.

• Bulletin of the Korean Chemical Society
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• 제25권10호
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• pp.1508-1512
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• 2004

A gas chromatography/mass spectrometric (GC/MS) method has been developed for the determination of trace mono-n-butyltin (MBT), di-n-butyltin (DBT), and tri-n-butyltin (TBT) compounds in sediments. Samples were extracted by 10% acetic acid in methanol containing 0.03% tropolone and were then derivatized for GC/MS analysis. Ethylation by sodium tetraethylborate and phenylation by sodium tetraphenylborate were evaluated as a derivatization reaction of the organotins in sample extract. n-Hexane was added into reaction media in the beginning of the reaction for the continuous extraction of derivatized organotins. Ethylation requires less than 2 hours to get proper derivatization yields for MBT, DBT, and TBT altogether and produces relatively low amounts of side reaction products. Compared to ethylation, phenylation requires much longer time but provides relatively lower yield and produces considerable amounts of side reaction products. Therefore, the ethylation reaction was applied for the analysis of organotin compounds in sediment. An isotope dilution mass spectrometric (IDMS) method based on GC/MS has been applied to the accurate determination of DBT compounds in the sediments. The IDMS results from the analyses of sediment samples showed a reasonable repeatability and a good agreement with the values obtained by IDMS based on liquid chromatography/induced coupled plasma/mass spectrometry.

• 한국지역사회생활과학회지
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• 제22권4호
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• pp.615-621
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• 2011

This study was conducted to evaluate of the protection efficiency in each part of developed pesticide-proof clothes by repeated washings. We investigated the effect of repeated laundering on mechanical properties of pesticide-proof clothes (not washed vs 5 times washed). We also examined pesticide infiltration rate into the pesticide-proof clothes by repeated laundering. The patches(TCL paper, surface area 50cm2)were attached to the inside of pesticide-proof clothes(head, chest, right upper-arm, right forearm, left thigh, left calf, back) which subjects had dressed in during pesticide spraying. The patches were detached from working clothes after work. For the extraction of pesticide in pesticide-proof clothes, sonication was applied for 30 min with methanol. The gas chromatography/mass spectrometry (GC/MS) was applied to identify the pesticide component. The results of this study are as follows: The force strength, water-vapour resistance and surface wetting resistance of pesticide-proof clothes decreased 5 times more in washed clothes. The concentration of pesticide was the highest in the head area of pesticide-proof clothes. In seven parts of TLC paper attached to the pesticide proof clothes, the concentration of pesticide was higher in the left thigh. The penetration part and concentration of pesticide increased as washing was repeated. Therefore the conclusion which can be drawn from this study is this: protection efficiency of pesticide-proof clothes decrease by repeated washings.

• Archives of Pharmacal Research
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• 제29권6호
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• pp.514-519
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• 2006

A simple HPLC method using UV detection was developed and validated for the determination of levodropropizine (LDP) In dog plasma. The sample was prepared for injection using a liquid-liquid extraction method with 1-phenypiperazine as the internal standard. The mobile phase was methanol - diethylamine solution (0.05 M) (20:80, v/v, pH adjusted to 3.0 with $H_3PO_4$) with a detection wavelength of 240 nm. The limit of quantitation (LOQ) of LDP in a biological matrix was determined to be 25.25 ng/mL. The calibration curve was linear across the concentration range of 25.25 to 2020 ng/mL. The intra-day and inter-day precision values (CV%) were within 7% and accuracy (R.E. %) was within 6% of the nominal values for medium (252.5 ng/mL) and high (2020 ng/mL) LDP concentrations. For the LDP concentration at the LOQ, the intra-day and inter-day precision and accuracy were within 20% and 10%, respectively. The average absolute recovery for LDP was 70.28%. This method was successfully used to analyze plasma samples in a steady-state bioavailability study of a newly developed sustained-release LDP tablets (SR) using immediate-release tablets (IR) as the reference. The relative bioavailability of the SR was determined to be $106.3\;{\pm}\;12.8%$ (n=6). The $C_{max}$ of the SR was significantly lower (p<0.05), and the $t_{max}$ was significantly longer than that of the IR (p<0.05). The results of ANOVA and two one-sided tests indicated that the SR exhibited acceptable sustained release properties and was bioequivalent to the IR.

• Archives of Pharmacal Research
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• 제19권6호
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• pp.529-534
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• 1996

A high-performance liquid chromatographic (HPLC) assay has been developed for the determination of ketorolac in human serum using a new extraction method with a good recovery. Human serum samples (1.0 ml) spiked with known concentrations of ketorolac tromethamine and 10${\mu}g$ of ketoprofen as the internal standard (IS) were acidified with 200${\mu}l$ of 1 N HCl and extracted with 7 ml of n-hexane-ether (7:3 v/v). Extracts were centrifuged and organic layer was back-extracted with 400${\mu}l$ of 0.1% tromethamine solution. Twenty .mu.l of centrifuged aqueous layer was injected onto a reversed-phase octyl column and eluted with a mixture of acetonitrile, water, methanol, and triethylamine [35:55:10:0.1 (v/v), pH 3.0] at a flow rate of 1.0 ml/min. Ultraviolet detection of ketorolac and IS was carried out at 300 nm. The calibration curve obtained using peak area ratios showed a good linearity (in concentration range 10-150 ng/ml $r^2$=O.9944; in range 50-2000 ng/ml, r$^{2}$=0.9998). The mean intra-day accuracy and precision for this HPLC method were found to be 3.6 and 3.7%, respectively. The mean inter-day accuracy and precision were found to be 4.0 and 3.7%, respectively, in the concentration range 50-2000 ng/ml. The recovery of ketorolac from serum was 92.0 $({\pm}5.7)$ % at the concentration of 100 ng/ml. This method proved to be readily applicable to the assay of ketorolac in human serum.

• 분석과학
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• 제29권4호
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• pp.186-193
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• 2016

본 연구는 용규전초로부터 열수추출방법(SNL-W)으로 1차 추출하고 부틸알코올을 이용하여 분별추출을 통해 유기용매분획(SNL-W/B)과 수상분획(SNL-W/W)을 각각 획득하였다. 각 분획의 총 알칼로이드함량과 사포닌함량을 측정하였고 수상분획의 메탄올 용출물은 알칼로이드 성분으로 확인되었다. 꿀벌봉독을 쥐의 복막 비만세포에 처리하여 알러지 유발물질인 히스타민을 분비시키고, 용규의 알칼로이드성분으로 히스타민 분비에 대한 저해효과를 고찰하였다. 그 결과, 용규의 수용성 알칼로이드성분(SNL-W/W/M)은 꿀벌봉독으로 유발된 비만세포의 히스타민 분비에 대하여 강한 저해요인으로 작용하는 것을 확인하였다.