• Title/Summary/Keyword: spectroscopic analysis method

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Differentiation of Recurrent Rectal Cancer and Postoperative Fibrosis: Preliminary Report by Proton MR Spectroscopy (재발성 직장암과 수술 후 섬유화의 감별 진단: 수소 MRS에 의한 예비보고)

  • Jeon Yong Sun;Cho Soon Gu;Choi Sun Keun;Kim Won Hong;Kim Mi Young;Suh Chang Hae
    • Investigative Magnetic Resonance Imaging
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    • v.8 no.1
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    • pp.24-31
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    • 2004
  • Purpose : To know the differences of proton MR spectroscopic features between recurrent rectal cancer and fibrosis in post-operative period, and to evaluate the possibility to discriminate recurrent rectal cancer from post-operative fibrosis by analysis of proton MR spectra. Materials and Methods : We evaluated the proton MR spectra from 25 soft tissue masses in perirectal area that developed in post-operative period after operation for the resection of rectal cancer. Our series included 11 cases of recurrent rectal cancer and 14 of fibrotic mass. All cases of recurrent rectal cancer and post-operative fibrosis were confirmed by biopsy. We evaluated the spectra with an attention to the differences of pattern of the curves between recurrent rectal cancer and post-operative fibrosis. The ratio of peak area of all peaks at 1.6-4.1ppm to lipid (0.9-1.6ppm) [P (1.6-4.1ppm/P (0.9-1.6ppm)] was calculated in recurrent rectal cancer and post-operative fibrosis groups, and compared the results between these groups. We also evaluated the sensitivity and specificity for discriminating recurrent rectal cancer from post-operative fibrosis by analysis of $^1H-MRS$. Results : Proton MR spectra of post-operative fibrosis showed significantly diminished amount of lipids compared with that of recurrent rectal cancer. The ratio of P (1.6-4.1ppm)/P (0.9-1.6ppm) in post-operative fibrosis was much higher than that of recurrent rectal cancer with statistical significance (p < .05) due to decreased peak area of lipids. Mean (standard deviations of P (1.6-4.1ppm)/P (0.9-1.6ppm) in post-operative fibrosis and recurrent rectal cancer group were $2.71{\pm}1.48\;and\;0.29{\pm}0.11$, respectively. With a cut-off value of 0.6 for discriminating recurrent rectal cancer from post-operative fibrosis, both the sensitivity and specificity were $100\%$ (11/11, and 14/14). Conclusion : Recurrent rectal cancer and post-operative fibrosis can be distinguished from each other by analysis of proton MR spectroscopic features, and $^1H-MRS$ can be a new method for differential diagnosis between recurrent rectal cancer and post-operative fibrosis.

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Isolation and HPLC-DAD validation of xanthoangelol in Lespedeza bicolor extract (싸리나무 추출물의 Xanthoangelol 분리 및 HPLC-DAD 밸리데이션)

  • Woo, Hyun Sim;Kim, Yeong-Su;Oh, Yu Jin;Cho, Hae Jin;Song, Se-Kyu;Kim, Dae Wook
    • Korean Journal of Food Science and Technology
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    • v.52 no.1
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    • pp.26-30
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    • 2020
  • This study was undertaken to determine the characteristics of xanthoangelol, the major chalcone constituent derived from the extracts of different parts of Lespedeza bicolor. Xanthoangelol was isolated from the root extract using column chromatography and used as a standard for quantitative analysis. The structure of the isolated compound was established based on spectroscopic evidence. The HPLC-DAD method was validated for specificity, linearity, precision, accuracy, limit of detection, and limit of quantitation. The calibration curve of xanthoangelol had significant linearity (R2>0.9999). Limit of detection and limit of quantitation 0.018 and 0.059 ㎍/mL, respectively. The relative standard deviation values of precision test, and intra- and inter-day tests were less than 0.22 and 0.40%, respectively. In the recovery test, the accuracy ranged from 98.98-102.78% with RSD values less than 0.13%. The method validation parameters indicate the applicability of the HPLC method for quality control of food or drug formulations containing L. bicolor.

Nonstoichiometry and Characteristics of the Perovskite $Y_{1-x}A_xFeO_{3-y}$ (A = Ca, Sr) Systems (페롭스카이트 $Y_{1-x}A_xFeO_{3-y}$ (A = Ca, Sr)계의 비화학양론과 특성 연구)

  • Yo, Chul-Hyun;Lee, Seung-Hyun;Lee, Sung-Joo;Park, Sung-Ho
    • Journal of the Korean Chemical Society
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    • v.35 no.6
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    • pp.617-624
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    • 1991
  • Nonstoichiometric solid solutions of $Y_{1-x}A_xFeO_{3-y}$ (A = Ca, Sr) systems with perovskite structure were prepared for x = 0.00, 0.25, 0.50, 0.75 and 1.00 at 1200$^{\circ}C$ under atmospheric pressure, respectively. Crystallographic structures of the solid solutions of all compositions have been determined by the analysis of X-ray diffraction patterns. Reduced lattice volume of the $Y_{1-x}Ca_xFeO_{3-y}$ system was decreased with increasing x value and that of the $Y_{1-x}Sr_xFeO_{3-y}$ system was increased with increasing the x value. The mole ratios of $ Fe^{4+}$ to $ Fe^{3+}$, ${\tau}$, values in the solid solutions have been determined by Mohr salt's method of analysis and then the mixed valency was identified by Mossbauer spectroscopic analysis at 298 K. The y values were calculated from the x and ${\tau}$, and then nonstoichiometric chemical formulas were fixed. The conduction mechanism could be explained by hopping model of the conduction electrons between the mixed valence states.

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Content Analysis and Classification for Polygonati Odorati Rhizoma and Polygonati Rhizoma by Steroidal Saponin (Steroidal Saponin을 이용한 위유, 황정의 분류 및 함량 분석법 개발)

  • Kim, Sun-Gun;Shin, So-Young;Moon, Ye-Ji;Seo, Ji-Yoon;Kim, Ho-Kyoung;Whang, Wan-Kyunn
    • YAKHAK HOEJI
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    • v.54 no.6
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    • pp.441-448
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    • 2010
  • In present study, classification and quality control of Genus Polygonatum were developed using the isolated from Polygonati Odorati Rhizoma and Polygonati Rhizoma. 3 components were isolated from Butanol fractions of Polygonati Rhizoma, and 2 components were isolated from Hexane and Butanol fractions of Polygonati Odorati Rhizoma. All the components were obtained using silica gel and ODS column chromatography. The compounds were identified as adenosine, 14-hydroxylfurost-5-ene-3-O-${\beta}$-D-glucopyranosyl-($1{\rightarrow}2$)-O-${\beta}$-D-glucopyranosyl-($1{\rightarrow}4$)-O-${\beta}$-D-galactopyranosyl-26-O-${\beta}$-D-glucopyranoside, 22-O-methyl-14-hydrocxyfurost-5-ene-3-O-${\beta}$-D-glucopyranosyl-($1{\rightarrow}2$)-O-${\beta}$-D-glucopyranosyl-($1{\rightarrow}4$)-O-${\beta}$-Dgalactopyranosyl-26-O-${\beta}$-D-glucopyranoside, ${\beta}$-Sitosteryl-3-O-${\beta}$-D-D-glucopyranoside, 14-hydoxylfurost-5-ene-3-O-${\beta}$-Dglucopyranosyl-($1{\rightarrow}2$)-O-[${\beta}$-D-xylopyranosyl-($1{\rightarrow}3$)]-O-${\beta}$-D-glucopyranosyl-($1{\rightarrow}4$)-O-${\beta}$-D-galactopyranoside through physicochemical data, spectroscopic methods ($^1H$-NMR, $^{13}C$-NMR, Mass) according references. The quality control of genus Polygonatum were conducted using HPLC quantitative analysis of 14-hydroxylfurost-5-ene-3-O-${\beta}$-D-glucopyranosyl-($1{\rightarrow}2$)-O-${\beta}$-D-glucopyranosyl-($1{\beta}4$)-O-${\beta}$-D-galactopyranosyl-26-O-${\beta}$-D-glucopyranoside, 14-hydoxylfurost-5-ene-3-O-${\beta}$-D-glucopyranosyl-($1{\rightarrow}2$)-O-[${\beta}$-D-xylopyranosyl-($1{\rightarrow}3$)]-O-${\beta}$-D-glucopyranosyl-($1{\rightarrow}4$)-O-${\beta}$-D-galactopyranoside in 30 samples collected throughout Korea and China. This method provided a tool for standardization of mix or misusing the commercial Odorati Rhizoma and Polygonati Rhizoma. As a result, contained quantity of 14-hydroxylfurost-5-ene-3-O-${\beta}$-D-glucopyranosyl-($1{\rightarrow}2$)-O-${\beta}$-D-glucopyranosyl-($1{\rightarrow}4$)-O-${\beta}$-D-galactopyranosyl-26-O-${\beta}$-D-glucopyranoside was measured $0.008{\pm}0.006%$ and 14-hydoxylfurost-5-ene-3-O-${\beta}$-D-glucopyranosyl-($1{\rightarrow}2$)-O-[${\beta}$-D-xylopyranosyl-(13)]-O-${\beta}$-D-glucopyranosyl-($1{\rightarrow}4$)-O-${\beta}$-Dgalactopyranoside was measured $0.026{\pm}0.012%$.

Formation of New Thorium (IV) Complexes with Crown Ethers (새로운 Thorium (IV)-Crown Ether 착물형성)

  • Jung, Hak-Jin;Jung, Oh-Jin;Suh, Hyouck-Choon
    • Journal of the Korean Chemical Society
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    • v.31 no.3
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    • pp.258-270
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    • 1987
  • A series of new thorium nitrate complexes with crown ethers have been synthesized from the reaction of the hydrated thorium nitrate, with the appropriate crown ethers of different cavity sizes in various solvents such as methanol, ethanol, butanol, methylacetate, acetone, tetrahydrofuran and acetylacetone. CHN elemental analysis, ICPAS, thermal analysis and Karl-Fischer method have been used to characterize their compositions, and the spectroscopic methods of IR, UV, $^1H-NMR$, and X-ray diffraction have been employed to determine the structures and solvolysis phenomena of these complexes. and the electrical conductances were measured in DMSO, and water solvent. The solvolysis have been observed only in the complexes synthesized in acetylacetone solvent. In the solvated complexes of 15-crown-5 and 18-crown-6, the mole ratio of $Th^{4+}$: ligand : acetylacetone is found to be 1:1:1, but in the non-solvated complexes of 12-crown-4 and 15-crown-5, the mole ratios of Th:L are 1:2 and 2:3, respectively, and that in the complexes of both 18-crown-6 and dicyclohexano-18-crown-6 is 1:1. All complexes which were not solvated have shown $n{\to}{\sigma}^{\ast}$ electronic transitions of crown ether whereas complexes solvated have exhibited both $n{\to}{\sigma}^{\ast}$ of crown ether and $n{\to}{\pi}^{\ast}$ transitions of acac. The dissociation mole ratio of $Th^{4+}$ and nitrate ion is found to be 1:1 in aprotic solvent, and 1:4 in protic solvent like water.

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Isolation and quantitative analysis of metabolites from Scrophularia buergeriana and their hepatoprotective effects against HepG2 Cells (현삼 (Scrophularia buergeriana)에서 분리한 화합물의 함량분석 및 간세포 보호 효과)

  • Na, Hyeon Seon;Oh, Seon Min;Shin, Woo Cheol;Bo, Jeon Hwang;Kim, Hyoung-Geun;Yoon, Dahye;Yang, Seung Hwan;Lee, Young-Seob;Kim, Geum-Soog;Baek, Nam-In;Lee, Moon-Soon;Lee, Dae Young
    • Journal of Applied Biological Chemistry
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    • v.62 no.4
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    • pp.399-406
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    • 2019
  • The roots of Scrophularia buergeriana were extracted with 80% aqueous Methanol and the concentrates were partitioned into EtOAc, n-BuOH, and H2O fractions. The repeated silica gel or octadecyl SiO2column, and medium pressure liquid chromatographies for the n-BuOH fraction led to isolation of phenylethanoid glycosides and iridoid glycosides. The chemical structures of these compounds were determined as harpagoside (1), angoroside C (2), aucubin (3) and acetoside (4) based on spectroscopic analyses including nuclear magnetic resonance and MS. A simple and efficient HPLC with UV detection method for the simultaneous determination of the four compounds (1-4) has been developed and applied to their content determination in the S. buergeriana. The roots were extracted by 80% methanol, and the contents of 1, 2, 3, and 4 were determined to 11.5, 7.6, 41.2, and 4.8 mg/g, respectively. Additionally, angoroside C (2) and acetoside (4) exhibited hepatoprotective effect against ethanol-induced hepatotoxicity in HepG2 cell line.

Quantitative Determination of Marker Compounds in the Extracts of Camellia sinensis L. Sub-branches (Residual Products) by HPLC (HPLC에 의한 차나무 잔가지(부산물)의 추출물 내 지표 성분의 정량분석)

  • Lee, Min Sung;Im, Hyeon Jeong;Jeong, Hea Seok;Cho, Hae Jin;Woo, Hyun Sim;Oh, Yu Jin;Lee, Soo In;Kim, Hyun Chul;Ahn, Kyung Wan;Kim, Yeong Su;Kim, Dae Wook
    • Korean Journal of Medicinal Crop Science
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    • v.27 no.1
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    • pp.24-29
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    • 2019
  • Background: Camellia sinensis L.(CS) is a perennial evergreen species of plant whose leaves are used to produce tea. In this plant species, the parts used are the leaves, sub-branch parts are thrown out. Methods and Results: Ethanol extract of sub-branch parts was used for isolation of major compounds by column chromatography. Structures were identified as caffeine (1), (-)-epicatechin (2) and (-)-epicatechin gallate (3) by interpretation of spectroscopic analysis, including $^1H$- and $^{13}C$-NMR. High-performance liquid chromatography (HPLC) method was used to compare the quantitative level of marker compounds in various extraction solvents of sub-branch parts of CS. The content of caffeine, (-)-epicatechin, and (-)-epicatechin gallate in 30% ethanol extract showed higher value with $3.28{\pm}0.57mg/g$, $5.53{\pm}0.88mg/g$, and $1.29{\pm}0.24mg/g$, respectively. Conclusions: These results indicated that not only leaves parts but also sub-branch, could be a good source for the functional material and pharmaceutical industry.

Antitumor Activity and Nephrotoxicity of the Novel Platinum(II) Coordination Complex (새로운 Platinum (II) Complex [Pt (II)(trans-d-dach)(DPPE)] $(NO_3)_2$의 항암효과 및 신독성에 관한 연구)

  • Jung Jee-Chang;Lee Moon-Ho;Chang Sung-Goo;Rho Young-Soo
    • The Korean Journal of Pharmacology
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    • v.31 no.1 s.57
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    • pp.103-114
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    • 1995
  • Platinum coordination complexes are currently one of the most compounds used in the treatment of solid tumors. However, its use is limited by severe side effects such as renal toxicity. Our platinum-based drug discovery program is aimed at developing drugs capable of diminishing toxicity and improving antitumor activity. We synthesized new Pt (Ⅱ) complex analogue containing 1,2-diaminocyclohexane (dach) as carrier ligand and 1,2-bis(diphenylphosphino) ethane (DPPE) as a leaving group. Furthermore, nitrate was added to improve the solubility. A new series of [Pt(trans-ddach)(DPPE).$2NO_3(PC)$ was synthesized and characterized by their elemental analysis and by various spectroscopic techniques [infrared (IR), $^{13}carbon$ nuclear magnetic resonance (NMR)]. PC demonstrated acceptable antitumor activity aganist P388, L-1210 lymphocytic leukemia cells and SK=OV3 human ovarian adenocarcinoma cells, and significant. activity as compared with that. cisplatin. The toxicity of PC was found quite less than thar of cisplatin using MTT, $[^3H]$ thymidine uptake and glucose consumption tests in rabbit proximal tubule cells, human kidney cortical cells and human renal cortical tissues. Based on these results, this novel platinum compound represent a valuable lead in the development of a new anticancer chemotherapeutic agent capable of improving antitumor activity and low toxicity.

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PHOTOELECTRIC OBSERVATIONS AND UBVRI LIGHT CURVES ANALYSIS OF ALGOL (Algol의 광전측광관측과 UBVRI 광도곡선의 분석)

  • 정장해;이용삼;임조령;양감징
    • Journal of Astronomy and Space Sciences
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    • v.10 no.2
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    • pp.123-145
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    • 1993
  • UBVRi photometry of Algol was carried out from December of 1988 to March of 1991 at Chungbuk National University Observatory and a total of 3465 observations in U, B, V, R, I were obtained. Three times of primary minimum light of JDH el 2447898.0938, JEH el 2448265.1205 and JDH el 2448288.0598, and two secondary minimum light of JDH el 2447808.1014 and JDH el 2448275.146 were determined from our observations. We analyzed simultaneously the UBVRI light curves of the Algol system with the Wilson-Devinney method for the determination of the photometric parameters. Indivisual masses for the 3 components of Algol are derived as $m_1$=3.36, $m_2$=0.76, $m_3$=1.6 in solar mass and radii as $R_1$=2.97, $R_2$=0.76 in solar radinus using i=$82.{\circ}47$, q=0.227, $r_1$=0.2102, $r_2$=0.2512 of our solution and some parameters of the spectroscopic solution of Hill et al. (1971). Our results is simiar to those reported by Kim (1989). The temperature of Algol C, $T_3$=8800 was obtained by means of fitting $l_1$, $l_2$, and $l_3$ of five colors to Planckian curve, and $R_3$=$1.6R_\odot$ is derived from its result. It is believed that its semidetached configuration of Algol A and B is the consequence of case B mass transfer. According to its location in a mass-radius diagram. Algol b may have evolved significantly in its Hburnning phase.

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A New Class of Platinum (II) Complexes [Pt (trans-1-daeh) (DPPP)] $2NO_3$ and [Pt (trans-1-daeh)(DPPE)] $2NO_3$ Exhibiting Antitumor Activity and Nephrotoxieity (새로운 Platinum (II) Complex ([Pt (II)(trans-1-dach)(DPPP)] $(NO_3)_2$와 [Pt (II)(trans-1-dach)(DPPE)] $(NO_3)_2$의 항암효과 및 신독성에 관한연구)

  • Jung, Jee-Chang;Yoon, Chin-Hee;Chang, Sung-Goo;Lee, Kyung-Tae;Rho, Young-Soo
    • The Korean Journal of Pharmacology
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    • v.29 no.2
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    • pp.283-295
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    • 1993
  • Pt-complexes is currently one of the most compounds used in the treatment of solid tumors. However, its used is limited by severe side effects such as renal toxicity. Our platinum-based drug discovery program is aimed at developing drugs capable of diminishing toxicity and improving antitumor activity. We synthesized new Pt (II) complex analogues containing 1, 2-diaminocyclohexane (dach) as carrier ligand and 1, 3-bis (diphenylphosphino) propane (DPPP)/1,2-bis (diphenylphosphino) ethane (DPPE) as a leaving group. Furthermore, nitrate was added to improve the solubility. A new series of (KHPC-001) [Pt (trans-1-dach)(DPPP)] $2NO_3$ and (KHPC-002) [Pt (trans-1-dach)(DPPE)] $2NO_3$ were synthesized and characterized by their elemental analysis and by various spectroscopic techniques [infrared (IR), $^{13}carbon$ nuclear magnetic resonance (NMR)]. KHPC-001 and KHPC-002 demonstrated acceptable antitumor activity aganist P-388, L-1210 lymphocytic leukemia cells and significant activity as compared with that of cisplatin. The toxicity of KHPC-001 and KHPC-002 was found quite less than that of cisplatin using MTT, $[^3H]$ thymidine uptake and glucose consumption tests in rabbit proximal tubule cells and human kidney cortical cells.

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