• Title/Summary/Keyword: 크로마토그래피

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Phospholipids Isolation from Squid Viscera Residues After Supercritical Carbon Dioxide Extraction (오징어 내장의 초임계 이산화탄소 추출 잔류물로부터 인지질의 분리)

  • U, Pyoung-Ook;Chun, Byung-Soo
    • Korean Chemical Engineering Research
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    • v.48 no.6
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    • pp.741-746
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    • 2010
  • Phospholipids were recovered from squid viscera residues by ethanol extraction after supercritical carbon dioxide($SCO_2$) extraction and from squid viscera was not processed $SCO_2$ by various organic solvent extraction. $SCO_2$ extraction were performed at $45^{\circ}C$ and 20 MPa for removal of non polar lipid molecules from freeze dried squid viscera sample. Phospholipids were extracted from freeze dried squid viscera sample by chloroform, hexane, methanol, and ethanol and from $SCO_2$extracted squid viscera sample by ethanol. The pH was fixed at 5.7 for all phospholipids extraction conditions. Phospholipid classes were analyzed by HPLC equipped with evaporative light scattering detector (ELSD). Phosphatidyl choline(PC) extracted by ethanol from $SCO_2$ extracted residues was higher than that of extracted by ethanol from squid viscera. But phosphatidyl ethanolamine(PE) and phosphatidic acid(PA) were extracted higher percentage in raw squid viscera. The fatty acid compositions in phospholipids extract by ethanol extract from $SCO_2$ extracted residues were analyzed by gas chromatography(GC). Docosahexanoic acid(DHA) was found in highest percentage in phospholipid extract.

A Study of the Retention Mechanism of the Monosubstituted Benzenes in Reversed-phase Liquid Chromatography (II) (역상 액체크로마토그래피에서 벤젠 일치환체들의 머무름 메카니즘에 관한 연구 (제 2 보))

  • Lee, Dai-Woon;Choi, Yong-Wook;Lee, Won
    • Journal of the Korean Chemical Society
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    • v.32 no.2
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    • pp.135-143
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    • 1988
  • The correlations between chromatographic parameters of monosubstituted benzenes and several physical parameters in reversed phase liquid chromatography were studied. The relationships between retention data and polarity index were investigated by plotting $log(log k'_S/k'_B)$ vs. $P'_S/P'_B$ which were relative retention and relative polarity index of monosubstituted benzenes with respect to benzene, respectively. The linear relationship between relative retention and polarity index was observed for the monosubstituted benzenes having polar group, while in case of those having nonpolar group, the good linearity was observed by combination with relative molecular weight i.e. $(P'_S/P'_B)/(MW_S/MW_B)$. Multivariant regression analysis, $a(P'_S/P'_B)+b(MW_S/MW_B)$+c did not give significantly better correlations compared to single variant analysis, $a[(P'_S/P'_B)/(MW_S/MW_B)]$+c, but multiple stepwise regression analysis was recommended when several physical parameters simultaneously were chosen. The best correlation between retention data for monosubstituted benzenes taken from the literature and substituent constant(${\pi}$), derived from hydrophobic parameter and the first order molecular connectivity index$(^1{\chi}^{\nu})$, was established for methanol/water mobile phase system. The larger the surface coverage of the stationary phase, the higher was the correlation coefficient between these two parameters and retention data.

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Development of Rapid and Simple Drug Identification and Semi Quantitative Analytical Program by Gas Chromatography-Mass Spectrometry (가스크로마토그래피/질량분석기를 이용한 약물의 확인 및 간이 정량분석 프로그램 개발)

  • Kim, Eun-Mi;Han, Eun-Young;Hong, Hyo-Jeong;Jeong, Su-Jin;Choe, Sang-Gil;Rhee, Jong-Sook;Jung, Jin-Mi;Yeom, Hye-Sun;Lee, Han-Sun;Lee, Sang-Ki
    • YAKHAK HOEJI
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    • v.55 no.2
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    • pp.106-115
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    • 2011
  • Systematic toxicological analysis (STA) means the process for general unknown screening of drugs and toxic compounds in biological fluids. In order to establish STA, in previous study we investigated pattern of drugs & poisons in autopsy cases during 2007~2009 in Korea, and finally selected 62 drugs as target drugs for STA. In this study, rapid and simple drug identification and quantitative analytical program by gas chromatography-mass spectrometry(GC-MS) was developed. The in-house program, "DrugMan", consisted of modified chemstation data analysis menu and newly developed macro modules. Total 55 drugs among 62 target drugs were applied to this program, they were 14 antidepressants, 8 anti-histamines, 5 sedatives/hypnotics, 5 narcotic analgesics, 3 antipsychotic drugs, and etc. For calibration curves, fifty five drugs were divided into four groups of range considering their therapeutic or toxic concentrations in blood specimen, i.e. 0.05~1 mg/l, 0.1~1 mg/l, 0.1~5 mg/l or 0.5~10 mg/l. Standards spiked bloods were extracted by solid-phase extraction (SPE) with trimipramine-D3 as internal standard. Parameters such as retention times, 3 mass fragment ions, and calibration curves for each drug were registered to DrugMan. A series of identification, semi quantitation of target drugs and reporting the results were performed automatically. Calibration curves for most drugs were linear with correlation coefficients exceeding 0.98. Sensitivity rate of DrugMan was 0.90 (90%) for 55 drugs at the level of 0.5 mg/l. For standard spiked bloods at the level of 0.5 mg/l for 29 drugs, semi quantitative concentrations were ranged 0.36~0.64 mg/l by DrugMan. If more drugs are registered to database in DrugMan in further study, it will be useful tools for STA in forensic toxicology.

Gas Chromatographic and Mass Spectrometric Determination of Alcohol Homologues in the Korean Folk Sojues (Distilled Liquor) (기체크로마토그래피 및 질량분석법에 의한 민속 소주중의 알코올 동족체 분석)

  • Lee, Dong Seon;Park, Hye Seong;Kim, Geon;Lee, Taek Su;No, Bong Su
    • Journal of the Korean Chemical Society
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    • v.38 no.9
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    • pp.640-652
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    • 1994
  • This work is undertaken to determine alcohol homologues so-called fusel oil that may be present in the Korean folk sojues (distilled liquor) made from grains and to describe sample preparation and analytical method by GC-FID-MS. Solid phase extraction method for sample preparation by using porous styrene divinyl benzene polymer (Porapak Q) was compared with steam distillation and solvent extraction method. Retention behaviors of homologous series of alcohols were also studied. Log values of retention time, molecular weight, boiling point, and capacity factor of alcohols showed linear correlations to the carbon number of an alcohol, to the oven temperature, and to the dielectric constant. Components such as methyl alcohol, n-propyl alcohol, isobutyl alcohol, isopentyl alcohol, and phenethyl alcohol have been identified. The more amount of isopentyl alcohol than other alcohols are contained in the Korean folk sojues, while that of n-propyl alcohol are contained in Chinese kaoliangchiew. Degree of similarity or dissimilarity and classification of the individual samples were discussed using multivariate statistical analysis(principal components analysis) based on GC data.

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Identification of catalytic acidic residues of levan fructotransferase from Microbacterium sp. AL-210 (Microbacterium sp. AL-210이 생산하는 levan fructotransferase의 효소활성에 중요한 아미노산의 동정)

  • Sung, Hee-Kyung;Moon, Keum-Ok;Choi, Ki-Won;Choi, Kyung-Hwa;Hwang, Kyung-Ju;Kim, Myo-Jung;Cha, Jae-Ho
    • Journal of Life Science
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    • v.17 no.1 s.81
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    • pp.6-11
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    • 2007
  • [ $\beta$ ]-Fructofuranosidases, a family 32 of glycoside hydrolases (GH32), share three conserved domains including the W(L/M)(C/N)DP(Q/N), FRDPK, and ECP(D/G) motifs. The functional role of the conserved acidic residues within three domains of levan fructotransferase, one of the $\beta-fructofuranosidases$, from Microbacterium sp. AL-210 was studied by site-directed mutagenesis. Each mutant was overexpressed in E. coli BL21(DE3) and purified by using Hi-Trap chelating affinity chromatography and fast performance liquid chromatography. Substitution of Asp-63 by Ala, Asp-195 by Asn, and Glu-245 by Ala and Asp decreased the enzyme activity by approximately 100-fold compared to the wild-type enzyme. This result indicates that three acidic residues Asp-63, Asp-195, and Glu-245 play a major role in catalysis. Since the three acidic residues are present in a conserved position in inulinase, levanase, levanfructotransferase, and invertase, they are likely to have a common functional role as nucleophile, transition state stabilizer, and general acid in $\beta-fructofuranosidases$.

Purification and Characterization of the Bacteriocin Produced by Lactococcus sp. KD 28 Isolated from Kimchi (김치에서 분리한 Lactococcus lactis가 생산하는 박테리오신의 정제 및 특성)

  • Lee, Ji-Young;Choi, Nack-Shick;Chun, Sung-Sik;Moon, Ja-Young;Kang, Dae-Ook
    • Journal of Life Science
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    • v.25 no.2
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    • pp.180-188
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    • 2015
  • The bacterial strain isolated from Kimchi showed antibacterial activity against Micrococcus luteus IAM 1056. The selected strain was identified as Lactococcus lactis by 16S rRNA nucleotide sequence analysis and named as Lactococcus sp. KD 28. The treatment of culture supernatant with proteinase K removed antibacterial activity, indicating its proteinaceous nature, a bacteriocin. This bacteriocin was sensitive to hydrolytic enzymes such as ${\alpha}$-chymotrypsion, trypsin, proteinase K, lipase, ${\alpha}$-amylase and subtilisin A. The bacteriocin was highly thermostable and resistant to heating at $80^{\circ}C$ for up to an hour but 50 % of the total activity was remained at $100^{\circ}C$ for 30 min. The pH range from 2.0 to 8.0 had no effect on bacteriocin activity and it was not affected by solvents such as acetonitrile, isopropanol, methanol, chloroform and acetone up to 50% concentration. The bacteriocin showed antibacterial activity against M. luteus IAM 1056, Lactobacillus delbrueckii subsp. lactis KCTC 1058, Enterococcus faecium KCTC 3095, Bacillus cereus KCTC 1013, B. subtilis KCTC 1023, Listeria ivanovii subsp. ivanovii KCTC 3444, Staphylococcus aureus subsp. aureus KCTC 1916, B. megaterium KCTC 1098 and B. sphaericus KCTC 1184. The bacteriocin was purified through ammonium sulfate concentration, SP-Sepharose chromatography and RP-HPLC. The molecular weight was estimated to be about 3.4 kDa by tricine-SDS-PAGE analysis.

Assessments of the VOCs and Smells Compounds Emitted from Properties Exhumed at Sim Seol Tomb (심설(沈偰)묘 출토유물에서 발현되는 VOCs 및 냄새물질의 특성 평가)

  • Seo, Yong-Soo;Lee, Young-Eun
    • Journal of Conservation Science
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    • v.28 no.1
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    • pp.63-73
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    • 2012
  • In this study, the 89 components of the gases emitted from grave goods at Sim Seol(1570-1630) tomb identified and quantitatively analyzed using a thermal desorption system integrated with gas chromatography-mass spectrometer. The concentration of major components show the levels of alpha-pinene 4,113ppbv, beta-pinene 2,510ppbv and limonene 2,424ppbv, that of the others orderly show p-menth-2-ene, acetone, isolongifolene and isoborneol. The functional groups of high concentration level cover 65% of terpenes and 25.8% of alcohols. The expected odor intensity orderly show 35.1% of terpenes, 33.4% of aldehydes and 8.8% of alcohols. Terpenes have generally effect of a perfume, antifungal and antimicrobial activity, and could come out of the pine(Pinus densiflora) coffin, aldehydes and alcohols could be come out of both the Sim Seol mirra and Pinus densiflora for a long time. The analyses of gases emitted from a excavated properties or a tomb are assessed that it can pc001 provide a scientific basis on a counterplan against harmful gases, a method of conservation treatments and a evaluation of effectiveness in conservation of cultural properties in a tomb.

Study on Qualitative Analysis for Lacquer Mixed with Some Additives by Pyrolysis‐Gas Chromatography/Mass Spectrometry (Py-GC/MS 분석법을 이용한 첨가물 혼합 옻칠 접착제의 정성분석)

  • Kim, Ji Eun;Yu, Ji A;Chung, Yong Jae
    • Journal of Conservation Science
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    • v.33 no.1
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    • pp.51-59
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    • 2017
  • Lacquer has been used as a natural paint or adhesive in Korea since 2nd century B.C. It has been found to have been used as an adhesive as mentioned in old records and as seen in excavated relics, It was also mixed with flour, animal glue, or fish glue to produce lacquer adhesives. Qualitative analysis and evaluation of the applicability of lacquer and additives was performed in this study. The results of EGA analysis for lacquer additives confirmed that the pyrolysis temperature of lacquer, glucose glue, and animal glue. On the basis of this result, raw lacquer sample was checked that pyrolysis product that originated from urushiol side chain (R group). Components originating from glucose and amino acid were detected in glutinous rice paste and animal glue samples. In this study, the optimum pyrolysis temperature for each lacquer and additive mixture was determined from basic qualitative analysis data. By performing the qualitative analysis of each mixture, the applicability of this technique for analyzing real relics was evaluated.

Utilization of [6]-gingerol as an origin discriminant marker influencing melanin inhibitory activity relative to its content in Pinellia ternata (반하(Pinellia ternata)에서의 [6]-gingerol 함량과 멜라닌 저해 활성에 영향을 미치는 원산지 판별 마커로의 활용)

  • An, Ju Hyeon;Won, Hyo Jun;Seo, Soo-Kyung;Kim, Doo-Young;Ku, Chang-Sub;Oh, Sei-Ryang;Ryu, Hyung Won
    • Journal of Applied Biological Chemistry
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    • v.59 no.4
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    • pp.323-330
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    • 2016
  • Pinellia ternata Breitenbach, the natural medicinal plant of the Araceae family, is a perennial plant originated from the East Asia, but also widely distributed in Europe and North America. Its tuber is used as traditional medicine for treatment of various diseases such as vomiting, inflammation, and traumatic injury. Pharmacological studies revealed that P. ternata possesses anticonvulsant, anti-tumor, insecticidal, and cytotoxic activities. Despite being well-known as the useful medicinal plant, there is no reliable, standardized method for origin discrimination. Ultra performance liquid chromatography-photodiode array detector and quadrupole time of flight-mass spectrometry based metabolite-profiling was applied to explore significant metabolite for origin discrimination between Korean and Chinese P. ternata. One compound was isolated from Korean P. ternata using repeated ODS column chromatography by bioactivity guided fractionation, and determined as [6]-gingerol according to the results of spectroscopic data including nuclear magnetic resonance and MS. This compound was selected as cosmeceutical biomarker by fingerprints, and it was associated to melanin inhibitory effect determining its origin authenticity. Furthermore, the calibration curve of biomarker was prepared using validated method for the comparison of content between Korean and Chinese P. ternata. This is the report to address the selection and successful validation of the discriminant metabolite for confirmation of Korean P. ternata.

High-Performance Liquid Chromatographic Determination of Phenothrin and Silafluofen Residues in Crops with Mass Spectrometric Confirmation (고성능 액체크로마토그래피와 질량분석법을 이용한 농산물 중 Phenothrin 및 Silafuofen의 정밀 잔류분석법 개발)

  • Lee, Young-Deuk;Oh, Jae-Ho;Jang, Sang-Won
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.389-400
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    • 2011
  • A high-performance liquid chromatographic (HPLC) method was developed to determine residues of phenothrin and silafluofen, known as synthetic pyrethroids, in agricultural commodities. Insecticide residues were extracted with acetone from representative samples of four crops which comprised rice, apple, pepper and cabbage. The extract was purified serially by liquid-liquid partition and Florisil column chromatography. For rice and pepper samples, acetonitrile/n-hexane partition was additionally adopted to remove nonpolar interferences. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate two phenothrin isomers and silafluofen from sample co-extractives. Intact parent compounds were sensitively detected by ultraviolet absorption at 226 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine phenothrin and silafluofen residues at 0.02 and 0.01 mg/kg, respectively. Mean recoveries of phenothrin and silafluofen from four crop samples fortified at three levels in triplicate were in the range of 82.4~109.8% and 83.7~109.8%, respectively. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types and spiking levels. A selected-ion monitoring (SIM) LC/mass spectrometry (MS) with electrospray ionization was provided to confirm the suspected residue of phenothrin, even though no sufficient ionization of silafluofen was obtained. Both phenothrin and silafluofen could be successfully confirmed by gas chromatography/MS SIM with electron impact at 70 eV. The proposed method is sensitive, repeatable and rapid enough to apply to officially routine inspection of agricultural products.