• Title/Summary/Keyword: Elution development

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Quantitative Analysis and Varietal Difference of Cyanidin 3-glucoside in Pigmented Rice

  • Park, Sun-Zik;Lee, Jong-Hoon;Han, Sang-Jun;Kim, Hong-Yeol;Ryu, Su-Noh
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.43 no.3
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    • pp.179-183
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    • 1998
  • The cyanidin 3-glucoside (C3G) extracted from pigmented rice seeds in 0.5% TFA (Trifluoro acetic acid) -95% ethanol was separated by High Performance Liquid Chromatography (HPLC). A HPLC system using a Develosil ODS-5 column and 0.1 % TFA-$H_2O$~0.1 % TFA-$CH_3CN$ gradient elution was selected for separation and quantitative determination of C3G. Regression equation obtained for the standard content of C3G pigment was as Y=21.95293$^*$X-14.726771 (r=0.99$^{**}$). Using this method, 326 domestic and introduced collections were evaluated for the C3G content. The Korean bred cultivar 'Heugjinjubyeo', showed highest C3G content (552 mg/100g seed) among the tested cultivars. Among the pigmented rice cultivars ten cultivars were selected for containing a high content of C3G. The content of C3G per 100g seeds was in high order as follows: Heugjinjubyeo (552mg)>Cheng Chang (321mg)>Kilimgeugmi (240mg)>PI160979-2 (224mg)>Hong Shei Lo (221mg)>Heugnambyeo (191 mg)>Mitak =PIl60979-1 (186mg)>Suwon425 (163mg)>Sanghaehyanghyeolla (108mg). The C3G pigment was not detected in the common white rice cultivars.

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Purification of Vasopressin-related Peptide, [Arg8]-vasotocin, from the Brain of Conger Eel (Conger myriaster) (붕장어 (Conger myriaster)의 뇌로부터 Vasopressin-related Peptide, [Arg8]-vasotocin의 정제)

  • Go Hye-Jin;KIM Chan-Hee;KIM Eun Jung;KIM In Hye;PARK Hee Yeon;YOON Ho Dong;HONG Yong-Ki;PARK Nam Gyu
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.38 no.1
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    • pp.6-11
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    • 2005
  • Vasopressin (VP)-related peptide was purified from the brain extract of conger eel (Conger myriaster) by reverse-phase, ion-exchange high performance liquid chromatography (HPLC). This peptide with a molecular weight of 1,051.2 Da was determined as $H-Cys-Tyr-Ile-Gln-Asn-Cys-Pro-Arg-Gly-NH_2$, whose Cys residues made an intramolecular disulfide bridge by the automated amino acid sequence analysis, MALDI- TOF mass spectrometry. It's sequence was confirmed by identity of the elution position with the synthetic peptide in HPLC system. As a result of homology investigation, the primary structure of this peptide was the same as that of VP-superfamily member, $[Arg^8]-vasotocin$. The synthetic peptide showed a contractile activity at a minimal effective concentration of $10^{-10}\;M$ on the intestinal smooth muscle of goldfish.

Determination of Isomaltooligosaccharides in Yoghurts by Using HPLC-ELSD (HPLC-ELSD를 이용한 발효유 제품 중의 Isomaltooligosaccharides 분석법 개발)

  • Ko, Jinhyouk;Lee, Moon-Seok;Kwak, Byung-Man;Ahn, Jang-Hyuk;Park, Jong-Su;Kwon, Joong-Ho
    • Food Science of Animal Resources
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    • v.33 no.3
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    • pp.417-424
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    • 2013
  • A rapid and simple analytical method for the determination of 9 isomaltooligosaccharides (IMO) species in yoghurts was developed using dispersive solid phase extraction (dSPE) clean-up technic and high performance liquid chromatography with evaporative light-scattering detector (HPLC-ELSD). In this study, 9 IMO were extracted from samples simply with chemical reagent using ISO22662 IDF198 method and additional dSPE clean-up. The optimum instrument conditions for the determination were used carbohydrate ES $5{\mu}$ column with gradient elution of water and acetonitrile and ELS detector. The linearity of this method was expressed as the correlation coefficient ($r^2$), the results of IMO 9 species were shown in 0.9999. LOD and LOQ were respectively 7.9-22.1 mg/kg, 25.9-72.8 mg/kg. The accuracy of intra- and inter-day measurements were in the range from $84.3{\pm}4.5$ to $104.9{\pm}6.5%$, and the preceision of the intra- and inter-day measurements were in the range from 0.8 to 7.7%. The recoveries were from $84.3{\pm}4.5$ to $104.9{\pm}6.5%$. The determination results of IMO 9 species for the 9 yoghurts circulated in the market were in the range from $0.317{\pm}0.007$ to $1.624{\pm}0.050$ g/100 g. The newly developed method is appropriate for the determination of IMO in yoghurts, is a rapid and simple method with excellent resolution in compared with previous method.

Effects of Activator on Rubber Characteristics for Gasket to Lithium Ion Battery (리튬 이온 전지용 개스킷 고무 물성에 미치는 가교조제의 영향)

  • Kang, Dong-gug;Kim, Hye-young;Kang, Young-im;Hur, Byung-ki;Seo, Kwan-ho
    • Applied Chemistry for Engineering
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    • v.22 no.4
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    • pp.395-399
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    • 2011
  • Material of the gasket for lithium ion battery requires the chemical resistance, the electrical insulting property, the compression set, the anti-contamination level and the low temperature resistance. We compounded ethylene propylene diene monomer (EPDM), which showed widely different solubility parameter index, with adjusting the amount of metal oxide as an activator. We did long-term test and compression set against an electrolyte with consideration for operating conditions in lithium-ion battery. In these tests, we checked the physical, chemical characteristics and the effect to lithium ion battery with different kinds of activators. In case of rubber with ZnO as an activator, through 1000 h depositing test in propylene carbonate which is one of representative solvents, we could get the satisfying characteristics and result. However, $Zn^{2+}$ had eluted in the ion elution test. So, ZnO should be limited in EPDM compound for the gasket material in lithium-ion battery.

Development of HPLC method for differentiation of three parts of mulberry tree

  • Eom, Ji Hyun;Vu, Thi Phuong Duyen;Cai, Linxi;Zhao, Yan;Li, Hong Xu;Yang, Seo Young;Kim, Young Ho;Kim, Seok Jin;Cho, Hyun So;Bao, Haiying;Chem, Jianbo;Kim, Kyung Tae;Kang, Jong Seong
    • Analytical Science and Technology
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    • v.30 no.3
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    • pp.130-137
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    • 2017
  • The leaves (Mori Folium; MF), branches (Mori Ramulus; MR), and root bark (Mori Cortex Radicis; MCR) of the mulberry tree have been used as therapeutic herbs for centuries. Existing analytical methods were developed specifically for different parts of the tree and cannot be applied to samples containing a mixture of tree parts. Such method specialization is time-consuming and requires separate identification and quality control of each tree part. This report describes an HPLC method for the simultaneous quality control and discrimination of MF, MR, and MCR using four marker compounds: rutin, kuwanon G, oxyresveratrol, and morusin. An Optimapak $C_{18}$ column ($4.6{\times}250mm$, $5{\mu}m$) was used with a gradient elution of 0.1 % formic acid in water and acetonitrile. The flow rate was 1.0 mL/min and the detection wavelength was 270 nm. In quantitative analyses of the three parts, rutin (0.11 % w/w) was detected only in MF. The oxyresveratrol content (0.12 % w/w) was highest in MR. Kuwanon G (0.33 % w/w) and morusin (0.18 % w/w) were higher in MCR than in other parts. The HPLC method given herein can be used to simultaneously classify and quantify three herbal medicines from the mulberry tree.

Analytical Method for the Validation of Hispidulin as a Marker Compound for the Standardization of Salvia plebeia R. Br. Extracts as a Functional Ingredient (배암차즈기 추출물의 기능성원료 표준화를 위한 지표성분으로서 Hispidulin의 분석법 평가)

  • Jeon, Yoon Jung;Kwak, Hoyoung;Choi, Jong Gil;Lee, Je Hyuk;Choi, Soo Im
    • Korean Journal of Medicinal Crop Science
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    • v.24 no.4
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    • pp.271-276
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    • 2016
  • Background: In the present study, we established an HPLC (high performance liquid chromatography)-analysis method for the determination of marker compounds as a part of the material standardization for the development of health-functional foods from Salvia plebeia R. Br. extract. Methods and Results: The quantitative determination method of hispidulin as a marker compound was optimized by HPLC analysis using a YMC hydrosphere C18 column with a gradient elution system. This method was validated using specificity, linearity, accuracy, and precision tests. It showed a high linearity in the calibration curve with a coefficient of correlation ($r^2$) of 0.999995. The method was fully validated, and was sensitive, with the limit of detection (LOD) at $0.09{\mu}g{\cdot}m{\ell}^{-1}$ and limit of quantification (LOQ) at $0.27{\mu}g{\cdot}m{\ell}^{-1}$. The relative standard deviation (RSD) values of the data from intra- and inter-day precision were 0.05 - 0.22% and 0.32 - 0.42%, respectively, and the intra- and inter-day accuracy of hispidulin were 99.5 - 102.3% and 98.8 - 101.5%, respectively. The average content of hispidulin in Salvia plebeia R. Br. extract was $3.945mg{\cdot}g^{-1}$ (0.39%). Conclusions: These results suggest that the developed HPLC method is very efficient, and that it could contribute to the quality control of Salvia plebeia R. Br. extracts as a functional ingredient in health functional foods.

Development of New Analytical Method of Vitamins Using Supercritical Fluid (초임계 유체를 이용한 비타민류의 새로운 분석법 개발)

  • Pyo, Dongjin;Park, Dongjin;Kim, Hohyun;Lee, Hakju;Lee, Taejoon
    • Analytical Science and Technology
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    • v.10 no.2
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    • pp.131-138
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    • 1997
  • Supercritical Fluid Chromatography(SFC) has become a technique for solving problems that are difficult to be monitored by other chromatographic methods. However, the most widely used fluid, is no more polar than hexane. Polar samples which are difficult to be analyzed with pure supercritical $CO_2$ because of their high polarity can be separated by adding polar modifiers to supercritical $CO_2$. In this paper, a new method for monitoring the mobile phase composition in modified supercritical fluid chromatography was developed. The amount of water dissolved in supercritical $CO_2$ was measured by amperometric microsensor which is made of thin film of perfluorosulfonate ionomer(PFSI). The amount of water dissolved in supercritical $CO_2$ stayed constant for a much longer time than with a saturator column. With this new mixing device, we could get good resolutions for vitamins which are difficult to separate with pure $CO_2$.

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Development of the testing method for vinyl chloride monomer (VCM) in polyvinyl chloride(PVC) samples (PVC 제품에서의 염화비닐 단량체 정량분석 방법에 관한 연구)

  • Kweon, Deok-Jun;Choi, Ki-In;Eom, Hui-Jeong;Lee, Jae-In;Choi, Zel-Ho
    • Analytical Science and Technology
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    • v.25 no.6
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    • pp.395-401
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    • 2012
  • This study presents a method for the quantitative analysis of residual vinyl chloride monomer (VCM) in PVC products. In elution solvent, the extraction efficiency was similar by ethanol, THF, and acetone, but using n-hexane, it indicated relatively low extraction efficiency. Measuring VCM in the pulverized PVC samples, it showed reasonable results in both the direct injection method and headspace method with GC/MS. Regarding analysis of VCM in the intermediate sponge samples, five laboratories showed good results, and from the results, it was considered that VCM quantitative method in this study was reliable.

Isolation and Characterization of an Acyclic Isoprenoid from Semecarpus anacardium Linn. and its Antibacterial Potential in vitro - Antimicrobial Activity of Semecarpus anacardium Linn. Seeds -

  • Purushothaman, Ayyakkannu;Meenatchi, Packirisamy;Saravanan, Nallappan;Karuppaiah, Muthu;Sundaram, Ramalingam
    • Journal of Pharmacopuncture
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    • v.20 no.2
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    • pp.119-126
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    • 2017
  • Objectives: Semecarpus anacardium Linn. is a plant well-known for its antimicrobial, antidiabetic and anti-arthritic properties in the Ayurvedic and Siddha system of medicine. This has prompted the screening of this plant for antibacterial activity. The main aims of this study were to isolate compounds from the plant's seeds and to evaluate their antibacterial effects on clinical bacterial test strains. Methods: The n-butanolic concentrate of the seed extract was subjected to thin layer chromatography (TLC) and repeated silica gel column chromatography followed by elution with various solvents. The compound was identified based on observed spectral (IR, $^1H$ NMR, $^{13}C$ NMR and high-resolution mass spectrometry) data. The well diffusion method was employed to evaluate the antibacterial activities of the isolated acyclic isoprenoid compound (final concentration: $5-15{\mu}g/mL$) on four test bacterial strains, namely, Staphylococcus aureus (MTCC 96), Bacillus cereus (MTCC 430), Escherichia coli (MTCC 1689) and Acinetobacter baumannii (MTCC 9829). Results: Extensive spectroscopic studies showed the structure of the isolated compound to be an acyclic isoprenoid ($C_{21}H_{32}O$). Moreover, the isoprenoid showed a remarkable inhibition of bacterial growth at a concentration of $15{\mu}g/mL$ compared to the two other doses tested (5 and $10{\mu}g/mL$) and to tetracycline, a commercially available antibiotic that was used as a reference drug. Conclusion: The isolation of an antimicrobial compound from Semecarpus anacardium seeds validates the use of this plant in the treatment of infections. The isolated compound found to be active in this study could be useful for the development of new antimicrobial drugs.

Comparative Analyses of Bioactive Constituents from Forsythia suspensa and Forsythia viridissima by HPLC-DAD

  • Won, Tae-Hyung;Liao, Lijuan;Lee, Seung-Ho;Son, Jong-Keun;Shin, Jong-Heon
    • Natural Product Sciences
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    • v.17 no.4
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    • pp.328-336
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    • 2011
  • A high-performance liquid chromatography (HPLC) with diode array detector (DAD) method was established for the discrimination of a folk medicine Forsythia suspensa and Forsythia viridissima. Five and three representative metabolites of the lignan and phenolic glycoside classes were selected for the analysis from F. suspensa and F. viridissima, respectively. The optimal chromatographic conditions were obtained on an ODS column (5 ${\mu}m$, $4.6{\times}250$ mm) with the column temperature at $40^{\circ}C$. The mobile phase was composed of methanol and 0.3% acetic acid using an isocratic elution with the flow rate 1 mL/min. Detection wavelength was set at 280 nm. All calibration curves showed good linear regression ($r^2$ > 0.996) within test ranges. Limits of detection (LOD) and limits of quantitation (LOQ) values were lower than 0.096 and 0.291 ${\mu}g/mL$, respectively. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.07-0.63% and 0.14-0.62%, respectively, and the overall recoveries of 97.79-102.46% for all of the compounds analyzed. In addition, effectiveness of diverse extraction methods was compared to each other for the development of standard analytical method. The verified method was successfully applied to the quantitative determination of representative metabolites in fifty-three commercial F. suspensa samples and fifteen commercial F. viridissima samples from diverse sources. The overall analytical results showed the unequivocal differences in bioactive constituents between F. suspensa and F. viridissima.