• 제목/요약/키워드: high performance liquid chromatography/mass spectrometry

검색결과 289건 처리시간 0.025초

Profiling Analysis of Sphingolipids in HL-60 Cells by High-Performance Liquid Chromatography-Tandem Mass Spectrometry in combination with Multiple Reaction Monitoring

  • Son, Jung-Hyun;Lee, Jae-Ick;Yang, Ryung;Kim, Dong-Hyun
    • 대한약학회:학술대회논문집
    • /
    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
    • /
    • pp.288.3-289
    • /
    • 2003
  • Sphingolipid species are important second messengers due to their role in the mitogenesis, differentiation and apoptosis. We developed a new column liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS) in combination with multiple reaction monitoring (MRM) method for the rapid, simultaneous and quantitative determination of unambiguous detecting sphingolipids in cell culture of human cancer cells (HL-60). (omitted)

  • PDF

Analysis of Carotenoids in 25 Indigenous Korean Coral Extracts

  • Kim, Sang Min;Kang, Suk-Woo;Lee, Eun A;Seo, Eun-Kyoung;Song, Jun-Im;Pan, Cheol-Ho
    • Journal of Applied Biological Chemistry
    • /
    • 제56권1호
    • /
    • pp.43-48
    • /
    • 2013
  • In this study, methanol extracts from 25 indigenous Korean corals were prepared and their carotenoid constituents were analyzed by high-performance liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (HPLC-APCI-MS). Among them, extracts from nine species showed detectable peaks in the HPLC chromatogram at 450 nm and the ultraviolet/visible spectra exhibiting carotenoid-specific characteristics were chosen. The mass data of carotenoid peaks revealed that only peridinin could be identified based on literature comparison and suggested the potential presence of novel carotenoid structures. This is the first reported investigation of indigenous Korean coral carotenoids and further work is needed to explore the carotenoids and their potential roles in the ecosystem of indigenous Korean corals.

Marker compounds contents of Salvia miltiorrhiza Radix depending on the cultivation regions

  • Seong, Gi-Un;Kim, Mi-Yeon;Chung, Shin-Kyo
    • Journal of Applied Biological Chemistry
    • /
    • 제62권2호
    • /
    • pp.129-135
    • /
    • 2019
  • Salvia miltiorrhiza Radix is cultivated in Korea and China and is traditionally used to treat cardiovascular diseases. In this study, we developed and validated a quantitative analysis method for S. miltiorrhiza Radix using high-performance liquid chromatography (HPLC). Identification was performed using ultra performance liquid chromatography-tandem mass spectrometry. For quantitative analysis, we used seven marker compounds. Separation conditions for HPLC were optimized using an ODS column with gradient conditions of 1% formic acid in distilled water and 1% formic acid in acetonitrile, with a flow rate of 0.8 mL/min and a detection wavelength of 280 nm. This method showed good linearity ($R^2=0.9998$), precision (relative standard deviation ${\leq}3.3%$), accuracy (recovery of 94.16-102.89%), limit of detection ($7.53{\mu}g/mL$), and limit of quantification ($23.71{\mu}g/mL$). This approach successfully quantified marker compounds in S. miltiorrhiza Radix. The individual marker compounds were identified by comparing the molecular masses and retention times with does standard compounds. Marker compound contents of S. miltiorrhiza Radix were investigated with different cultivation regions. Seven marker compounds were detected and quantified in all samples. Among them, salvianolic acid B showed the highest contents and it ranged from 4.13 to 7.15%. The salvianolic acid B content (7.15%) of marker compound was the highest in Bonghwa, and the tanshinone IIA content (1.90%) was the highest in Pohang. The results of marker compounds and developed method were intended to provide a favorable reference for the study of S. miltiorrhiza Radix from different regions of Korea.

Simultaneous Determination of Benzoic Acid, Caffeic Acid and Chlorogenic Acid in Seeds of Eriobotrya japonica and their Antibacterial Effect

  • Jeong, Jun-Mo;Lee, Kyoung-In;Kim, Sun-Min
    • Journal of Applied Biological Chemistry
    • /
    • 제57권1호
    • /
    • pp.89-93
    • /
    • 2014
  • We aim to develop a simple method for simultaneous and quantitative determination of benzoic acid, caffeic acid and chlorogenic acid in seeds of Eriobotrya japonica. In addition, antibacterial effect of these three phenolic acids was examined. A basic method is performed on the high performance liquid chromatography system coupled to an UV-detector (230 nm) and reverse phase C-18 column ($4.6{\times}150mm$, $5{\mu}m$). Each phenolic acid was confirmed via liquid chromatography-mass spectrometry (MS)/MS system under the multiple-reaction monitoring with negative-ion electrospray ionization (ESI(-)) mode. It is demonstrated that the method was could be applied to samples for an analytical study of the phenolic acids. On the other hand, three phenolic acids in seeds of E. japonica exhibited antibacterial effect against several pathogenic bacteria. Of these, benzoic acid was found to have stronger antibacterial effect.

Isolation and Structural Characterization of an Oligosaccharide Produced by Bacillus subtilis in a Maltose-Containing Medium

  • Shin, Kwang-Soon
    • Preventive Nutrition and Food Science
    • /
    • 제21권2호
    • /
    • pp.124-131
    • /
    • 2016
  • Among 116 bacterial strains isolated from Korean fermented foods, one strain (SS-76) was selected for producing new oligosaccharides in a basal medium containing maltose as the sole source of carbon. Upon morphological characterization using scanning electron microscopy, the cells of strain SS-76 appeared rod-shaped; subsequent 16S rRNA gene sequence analysis revealed that strain SS-76 was phylogenetically close to Bacillus subtilis. The main oligosaccharide fraction B extracted from the culture supernatant of B. subtilis SS-76 was purified by high performance liquid chromatography. Subsequent structural analysis revealed that this oligosaccharide consisted only of glucose, and methylation analysis indicated similar proportions of glucopyranosides in the 6-linkage, 4-linkage, and non-reducing terminal positions. Matrix-assisted laser-induced/ionization time-of-flight/mass spectrometry and electrospray ionization-based liquid chromatography-mass spectrometry/mass spectrometry analyses suggested that this oligosaccharide consisted of a trisaccharide unit with 1,6- and 1,4-glycosidic linkages. The anomeric signals in the $^1H$-nuclear magnetic resonance spectrum corresponded to ${\alpha}$-anomeric configurations, and the trisaccharide was finally identified as panose (${\alpha}$-D-glucopyranosyl-1,6-${\alpha}$-D-glucopyranosyl-1,4-D-glucose). These results suggest that B. subtilis SS-76 converts maltose into panose; strain SS-76 may thus find industrial application in the production of panose.

Analysis of oligosaccharides from Panax ginseng by using solid-phase permethylation method combined with ultra-high-performance liquid chromatography-Q-Orbitrap/mass spectrometry

  • Li, Lele;Ma, Li;Guo, Yunlong;Liu, Wenlong;Wang, Yang;Liu, Shuying
    • Journal of Ginseng Research
    • /
    • 제44권6호
    • /
    • pp.775-783
    • /
    • 2020
  • Background: The reports about valuable oligosaccharides in ginseng are quite limited. There is an urgent need to develop a practical procedure to detect and analyze ginseng oligosaccharides. Methods: The oligosaccharide extracts from ginseng were permethylated by solid-phase methylation method and then were analyzed by ultra-high-performance liquid chromatography-Q-Orbitrap/MS. The sequence, linkage, and configuration information of oligosaccharides were determined by using accurate m/z value and tandem mass information. Several standard references were used to further confirm the identification. The oligosaccharide composition in white ginseng and red ginseng was compared using a multivariate statistical analysis method. Results: The nonreducing oligosaccharide erlose among 12 oligosaccharides identified was reported for the first time in ginseng. In the comparison of the oligosaccharide extracts from white ginseng and red ginseng, a clear separation was observed in the partial least squares-discriminate analysis score plot, indicating the sugar differences in these two kinds of ginseng samples. The glycans with variable importance in the projection value large than 1.0 were considered to contribute most to the classification. The contents of oligosaccharides in red ginseng were lower than those in white ginseng, and the contents of maltose, maltotriose, maltotetraose, maltopentaose, maltohexaose, maltoheptaose, maltooctaose, maltononaose, sucrose, and erlose decreased significantly (p < 0.05) in red ginseng. Conclusion: A solid-phase methylation method combined with liquid chromatography-tandem mass spectrometry was successfully applied to analyze the oligosaccharides in ginseng extracts, which provides the possibility for holistic evaluation of ginseng oligosaccharides. The comparison of oligosaccharide composition of white ginseng and red ginseng could help understand the differences in pharmacological activities between these two kinds of ginseng samples from the perspective of glycans.

LC/MS에 의한 원료생강 및 생강 페이스트 중의 Gingerol 화합물 분석 (Analysis of Gingerol Compounds of Raw Ginger (Zingiber officinale Roscoe) and Its Paste by High Performance Liquid Chromatograph-Mass Spectrometry (LC/MS))

  • 조길석
    • 한국식품영양과학회지
    • /
    • 제29권5호
    • /
    • pp.747-751
    • /
    • 2000
  • 본 연구에서는 생각의 매운맛을 주요성분인 gingerol 화합물의 분석방법을 개선할 목적으로, 원료 생각을 아세톤으로 추출한 후 그 추출물을 TLC 및 LiChrosorb RP-18 column으로 장착된 HPLC를 사용하여 3가지 gingerol 동족체 화합물을 분리하였고, LC/MS 및 NMR로 확인한 결과 생강의 동족체 화합물은 [6]-, [8]-, [10]-gingerol로 확인되었다. 본 방법으로 추출한 gingerol 표준품을 사용하여 시판 원료생강 및 생각 페이스트 중의 gingerol 함량을 측정한 결과, 전자의 경우 [6]-, [8]-, [10]-gingerol 함량은 635.5 mg%, 206.6 mg%, 145.7 mg%이었고, 후자의 경우는 418.2 mg%, 142.6 mg%, 103.3 mg%로 각각 구성되어 있었다.

  • PDF

Determination of Polar Secondary Metabolomes in Arabidopsis thaliana using High Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry

  • Cho, Young-Ah;Park, Se-min;Bae, Dong-Won;Seo, On-Nuri;Lee, Ji-Eun;Jeong, Sung-Woo;Kwon, Young-Sang;Cha, Jae-Yul;Bae, Han-Hong;Shin, Sung-Chul
    • 농업생명과학연구
    • /
    • 제46권6호
    • /
    • pp.165-171
    • /
    • 2012
  • As a preceding study for investigating the influence of sound wave stimulus on Arabidopsis thaliana metabolomics, the polar secondary metabolomes of the plant were determined using high performance liquid chromatography coupled with tandem mass spectrometry. A total of 10 polar secondary metabolomes were characterized and quantified. Among them, 4 metabolomes, p-coumaroylagmatine isomer (7 and 8), p-coumaroylagmatine isomer (9 and 10) were identified in the plant for the first time. The validation was conducted in terms of linearity, recovery, precision, limit of detection (LOD) and limit of quantification (LOQ). The validated method was applied to the simultaneous quantification of the 10 polar secondary metabolomes.

Polyphenolic Profile of Fermented Houttuynia cordata Thunb. and Overall Contribution to Antioxidant and Lipolytic Activities

  • Lee, Soo Jung;Hu, Wensi;Lee, Eun Jung;Choi, Jin Young;Koo, Ok Kyung
    • 산업식품공학
    • /
    • 제22권4호
    • /
    • pp.295-303
    • /
    • 2018
  • Polyphenol profiles, physicochemical properties, antioxidant activities, and inhibitory effect of adipocyte differentiation of Houttuynia cordata fermented with Lactobacillus brevis B84 were evaluated. Six polyphenols were characterized for this plant by using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), and the results were compared with total phenolic content by a spectrophotometric method. The total amount of the identified polyphenols was lower than that determined by the spectrophotometric method. However, the fermentation process influenced polyphenol composition such as content of vanillic acid and caffeic acid. The phytochemical profiles were evaluated by high-performance liquid chromatography with UV and electrospray ionization mass spectrometry detection ($HPLC-DAD-ESI-MS^n$). Total sugar and reducing sugar contents decreased after fermentation. Antioxidant activities such as DPPH, ABTS, and superoxide anion radical scavenging and reducing power were evaluated to compare the beneficial effect after fermentation. Fermented H. cordata increased the lipolytic effect in 3T3-L1 adipocytes. Overall, the results indicate that the fermentation of H. cordata with L. brevis B84 produces changes of phenolic compounds, antioxidant activity, and lipolytic effect.

Application of Fast Atom Bombardment Collision-induced Dissociation Tandem Mass Spectrometry for Structural identification of Glycerolipids Isolated From Marine Sponge

  • Lee, Sun-Young;Hong, Joo-Yeon;Jung, Jee-H.;Hong, Jong-Ki
    • Mass Spectrometry Letters
    • /
    • 제2권1호
    • /
    • pp.8-11
    • /
    • 2011
  • Two types of glycerolipids [monoacylglycerols (MAG) and cyclitols] were isolated by reversed phase high-performance liquid chromatography from the methanol extracts of a marine sponge, and analyzed by fast atom bombardment mass spectrometry (FAB-MS) in positive-ion mode. FAB mass spectra of these compounds yielded protonated molecules $[M + H]^+$ and abundant sodiated molecules $[M + Na]^+$ from a mixture of 3-nitrobenzyl alcohol and NaI. The structures of these compounds were elucidated by FAB-collisional-induced dissociation (CID)-tandem mass spectrometry. We carried out collision-indused dissociation (CID) of these lipids in B/E-linked scan mode. The CID B/E-linked scan of $[M + H]^+$ and $[M + Na]^+$ precursor ions resulted in the formation of numerous characteristic product ions through a series of dissociative processes. The product ions formed by charge-remote fragmentation (CRF) provided important information for the identification of the acyl chain structure substituted at the glycerol backbone. Some of the product the ions were diagnostic for the presence of a glycerol backbone or acyl chain structure.