scholarly journals Laguncularia racemosa Phenolics Profiling by Three-Phase Solvent System Step-Gradient Using High-Performance Countercurrent Chromatography with Off-Line Electrospray Mass-Spectrometry Detection

Molecules ◽  
2021 ◽  
Vol 26 (8) ◽  
pp. 2284
Author(s):  
Fernanda das Neves Costa ◽  
Gerold Jerz ◽  
Peter Hewitson ◽  
Fabiana de Souza Figueiredo ◽  
Svetlana Ignatova
Keyword(s):  
Mass Spectrometry ◽  
High Performance ◽  
Gradient Elution ◽  
Solvent System ◽  
Laguncularia Racemosa ◽  
Phase System ◽  
Ionization Mass ◽  
Countercurrent Chromatography ◽  
Esi Ms ◽  
Three Phase

The detailed metabolite profiling of Laguncularia racemosa was accomplished by high-performance countercurrent chromatography (HPCCC) using the three-phase system n-hexane–tert-butyl methyl ether–acetonitrile–water 2:3:3:2 (v/v/v/v) in step-gradient elution mode. The gradient elution was adjusted to the chemical complexity of the L. racemosa ethyl acetate partition and strongly improved the polarity range of chromatography. The three-phase solvent system was chosen for the gradient to avoid equilibrium problems when changing mobile phase compositions encountered between the gradient steps. The tentative recognition of metabolites including the identification of novel ones was possible due to the off-line injection of fractions to electrospray ionization mass spectrometry (ESI-MS/MS) in the sequence of recovery. The off-line hyphenation profiling experiment of HPCCC and ESI-MS projected the preparative elution by selected single ion traces in the negative ionization mode. Co-elution effects were monitored and MS/MS fragmentation data of more than 100 substances were used for structural characterization and identification. The metabolite profile in the L. racemosa extract comprised flavonoids, hydrolysable tannins, condensed tannins and low molecular weight polyphenols.

Determination of a Yellow Rice Toxin, Luteoskyrin, in Rice by Using Liquid Chromatography–Tandem Mass Spectrometry with Electrospray Ionization

2009 ◽  
Vol 72 (6) ◽  
pp. 1321-1326 ◽  
Author(s):  
KOHEI MIZUTANI ◽  
SUSUMU KUMAGAI ◽  
NAOKI MOCHIZUKI ◽  
YASUSHI KITAGAWA ◽  
YOSHIKO SUGITA-KONISHI
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Electrospray Ionization ◽  
High Performance ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Phase System ◽  
Ionization Mass ◽  
Solid Phase Extraction Cartridge ◽  
Relative Standard

Penicillium islandicum produces luteoskyrin (LUT), a yellow rice toxin that has been found frequently in rice. However, conventional analytical methods for determining LUT are limited, are complicated, and exhibit low sensitivity. In this study, an analytical method more sensitive and simple based on high-performance liquid chromatography combined with electrospray ionization mass spectrometry was developed. The cleanup procedure of the method was one step, using a solid-phase extraction cartridge. An isocratic mobile-phase system, consisting of acetonitrile–water–acetic acid (50:49:1 [vol/vol/vol]) at a flow rate of 0.2 ml/min, was utilized to obtain the best resolution. Our method showed good linearity (r = 0.9993, 0.5 to 50 ng/g) and high repeatability (relative standard deviation = 8.9 and 5.1% at levels of 0.5 and 10 ng/g, respectively) in the fortification test. The detection and quantification limits for the method in multiple-reaction monitoring mode were 0.1 and 0.3 ng/g, respectively. The average recovery of LUT in spiked rice at 0.5 and 10 ng/g was 80.7 and 85.2%, respectively. The method developed in this study should be applicable to survey LUT in rice, with high sensitivity, selectivity, and rapidity.

scholarly journals A Rapid Determination and Quantification of Three Biologically Active Polyisoprenylated Benzophenones using Liquid Chromatography-Tandem Mass Spectrometry (MRM) Method in Five Garcinia species from Cameroon

2017 ◽  
Vol 12 (12) ◽  
pp. 1934578X1701201
Author(s):  
Bernadette Messi Biloa ◽  
Raimana Ho ◽  
Guillaume Marti ◽  
Alain Meli Lannang ◽  
Jean-Luc Wolfender ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Performance ◽  
Rapid Determination ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Biologically Active ◽  
Ionization Mass ◽  
Relative Standard

Following investigation of Garcinia genus, a sensitive, rapid and simple reversed-phase high performance liquid chromatography-electrospray ionization mass spectrometry method has been developed for the identification and quantification of three polyisoprenylated benzophenones, garcinol (1), isogarcinol (2) and 7- epi-clusianone (3), in the extracts of five Garcinia species from Cameroon. The separation of those compounds was achieved on a RP-18 column using a solvent system consisting of a mixture of acetonitrile-water-formic acid as a mobile phase in a gradient elution mode. The identification of the three compounds was determined on a triple quadripole mass spectrometer with ESI interface operating in the negative mode. A multiple reaction monitoring (MRM) method was developed for the quantification of these polyisoprenylated benzophenones in the extracts of the Garcinia species. The method was validated through intra- and inter-day precision, with the relative standard deviation (RSD) less than 6%, limits of detection (LOD) and limits of quantification (LOQ) <1 ng. Overall recoveries ranged from 94% to 104%, with RSDs ranging from 0.8% to 4.5%. The results indicated that the fruits of G. preussii and the roots of G. brevipedicellata are good source of garcinol (1) and isogarcinol (2) respectively.

scholarly journals The chemical composition of the floral extract of Epipogium aphyllum sw. (Orchidaceae): A clue for their pollination biology

2014 ◽  
Vol 66 (3) ◽  
pp. 989-998 ◽  
Author(s):  
Anna Jakubska-Busse ◽  
Izabela Jasicka-Misiak ◽  
Anna Poliwoda ◽  
Emilia Święczkowska ◽  
Paweł Kafarski
Keyword(s):  
Mass Spectrometry ◽  
Chemical Composition ◽  
High Performance ◽  
Floral Scent ◽  
Pollination Biology ◽  
Ionization Mass ◽  
Methyl Cinnamate ◽  
Esi Ms ◽  
Array Detection ◽  
Pollination Systems

Epipogium aphyllum is a rare European obligate mycoheterotrophic orchid lacking chlorophyll. It has not been studied previously with respect to pollination biology. We studied the association between the composition of floral scent emission and its pollination systems. Field observation indicates that the main pollinators of Epipogium aphyllum are representatives of the genus Bombus (Hymenoptera), B. lucorum, B. hortorum, B. terrestris, B. pascuorum and B. proteus, and the genus Apis (Hymenoptera) namely A. mellifera. The main potential vector (observed to accidentally carry pollen), is most likely Episyrphus balteatus (Diptera, Syrphidae). The chemical composition of the floral extracts of 4 populations of Epipogium aphyllum Sw. growing naturally in Poland and the Czech Republic was examined by gas chromatography coupled with mass spectrometry (GC-MS) and high-performance liquid chromatography coupled with diode-array detection and electrospray ionization mass spectrometry (LC-ESI-MS) techniques. According to GC-MS analysis, 9-tricosene, nonadecane, 1-nonadecene and nonacosane predominated in the floral extracts. The studied samples were also characterized by relatively high amounts of benzenoids, e.g. methyl cinnamate, which is known as an attractant to the males of various orchid bees. LC-ESI-MS revealed the presence of flavor compounds such as vanillin (4-hydroxy-3-methoxybenzaldehyde) and its derivative acetovanillone, together with higher amounts of aliphatic and phenolic acids. Additionally, we detected the presence of indole and morphine derivatives.

scholarly journals Pharmacokinetics and Tissue Distribution Study of Chlorogenic Acid from Lonicerae Japonicae Flos Following Oral Administrations in Rats

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Yulu Zhou ◽  
Ting Zhou ◽  
Qi Pei ◽  
Shikun Liu ◽  
Hong Yuan
Keyword(s):  
Mass Spectrometry ◽  
Oral Administration ◽  
Chlorogenic Acid ◽  
Tissue Distribution ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Gradient Elution ◽  
Tissue Homogenate ◽  
Ionization Mass

Chlorogenic acid (ChA) is proposed as the major bioactive compounds of Lonicerae Japonicae Flos (LJF). Forty-two Wistar rats were randomly divided into seven groups to investigate the pharmacokinetics and tissue distribution of ChA, via oral administration of LJF extract, using ibuprofen as internal standard, employing a high performance liquid chromatography in conjunction with tandem mass spectrometry. Analytes were extracted from plasma samples and tissue homogenate by liquid–liquid extraction with acetonitrile, separated on a C18 column by linear gradient elution, and detected by electrospray ionization mass spectrometry in negative selected multiple reaction monitoring mode. Our results successfully demonstrate that the method has satisfactory selectivity, linearity, extraction recovery, matrix effect, precision, accuracy, and stability. Using noncompartment model to study pharmacokinetics, profile revealed that ChA was rapidly absorbed and eliminated. Tissue study indicated that the highest level was observed in liver, followed by kidney, lung, heart, and spleen. In conclusion, this method was suitable for the study on pharmacokinetics and tissue distribution of ChA after oral administration.

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