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Authors: Feng Wu, Xiuli Zhao, Shumin Wang, Hui Zhou, Shaojie Guo, Siyang Ni, Bo Yang, Lihua Zhang and Xinde Xu

(Marietta, OH, USA). Human drug-free plasma was obtained from healthy volunteers, in accordance with the local ethics guidelines. Instrumentation The HPLC-MS/MS equipment consisted of an API-4000 mass spectrometry from AB

Open access
Authors: Filip Šibul, Dejan Orčić, Sanja Berežni, Goran Anačkov and Neda Mimica-Dukić

concentration of 200 mg/mL, for their storage [ 34 ]. Quantitative HPLC–MS/MS Analysis For quantitative determination of compounds in the examined extracts, the method for quantification of 45 plant phenolics by Orčić et al

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Authors: Jong-Woo Jeong, Yun-Hwan Seol, Hun-Chan Hyun, Hye-Rim Kim, Jong-Hwa Lee, Young-Dae Gong, Nam Sook Kang and Tae-Sung Koo

3. HPLC–MS/MS chromatograms of samples from (a) double blank rat plasma, (b) rat plasma containing supinoxin (1 ng mL −1 ) and DGG-200064 (1 μg mL −1 ), and (c) a rat plasma sample obtained 3 h after oral administration

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, Hopkinton, MA, USA). The dry residue was reconstituted with 100 μL of methanol, and a 5 μL aliquot was injected into the high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) system for analysis. HPLC-MS/MS analysis The LC

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A new, sensitive, and selective high-performance liquid chromatography-tandem mass spectrometric method (HPLC-MS/MS) has been developed for the quantification of six flavonoids (sophoricoside, genistin, genistein, rutin, quercetin, and kaempferol) in rat bile and urine. The sample pretreatment was simple by liquid-liquid extraction. Sulfamethalazole was used as internal standard (IS). During method development, the effect of extraction volume, mobile phase composition, column temperature, and injection volume were varied to optimize sensitivity and achieve a run time as short as possible. Chromatographic separation was accomplished on a C18 column with a simple linear gradient elution within 9 min. Full validation of the assay was in accordance with the requirement of the validation of the method in vivo and implemented including specificity, linearity, accuracy, precision, recovery, and matrix effect. This is the first report on determination of the major flavones in rat bile and urine after oral administration of Fructus Sophorae extract. The method has been used successfully in excretion studies of six major flavonoids in rat bile and urine.

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Authors: SeonJu Park, Nanyoung Kim, Jun Hyung Park, Sang-Won Lee, Jae-Hyoung Song, Hyun-Jeong Ko, Han-Jung Chae, Hyung-Ryong Kim and Seung Hyun Kim

spectrometry (HPLC–MS/MS) for the simultaneous determination of seven sesquiterpene lactone glucosides, namely, 11 β ,13-dihydrozaluzanin-3- O - β -glucopyranoside ( 1 ), ixerin F ( 2 ), macrocliniside A ( 3 ), 8-epiisolipidiol-3- O - β -glucopyranoside ( 4

Open access

Summary

A selective and sensitive liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) method was developed and validated for analysis of xanthotoxol (1), xanthotoxin (2), isoimpinellin (3), bergapten (4), oxypeucedanin (5), imperatorin (6), cnidilin (7), and isoimperatorin (8) in rat bile and urine using pimpinellin as an internal standard (IS). An Agilent 1200 liquid chromatography system (Agilent Technologies, USA) equipped with a quaternary pump, an autosampler, and a column compartment was used for all analyses. Chromatographic separations were performed on a Sapphire C18 column (150 mm × 4.6 mm, 5 μm), and the column temperature was maintained at 30°C; the sample injection volume was 10 μL. The specificity, linearity, accuracy, precision, recovery, matrix effect, and several stabilities were validated for all analytes in the rat bile and urine samples. The method was successfully applied in monitoring the concentrations of eight coumarins in rat bile and urine after a single oral administration of Radix Angelicae Dahuricae extract with a dosage of 8.0 mL/kg. In the bile samples, the eight coumarins excreted completely in twenty-four hours. The average percentages of coumarins (1–8) excreted were 0.045%, 0.019%, 0.177%, 0.105%, 0.337%, 0.023%, 0.024%, 0.021%. In the urine samples, the eight coumarins excreted completely in seventy-two hours. The average percentages of coumarins (1–8) excreted were 1.78%, 0.095%, 0.130%, 0.292%, 0.082%, 0.008%, 0.005%, 0.004%. The method is robust and specific and it can successfully complete the requirements of the excretion study of the eight coumarins in Radix Angelicae Dahuricae.

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Authors: Emil Mincsovics, Péter Ott, Ágnes Alberti, Andrea Böszörményi, Éva Héthelyi, Éva Szőke, Ágnes Kéry, Éva Lemberkovics and Ágnes Móricz

Bioassay-guided isolation of antibacterial components of chamomile flower methanol extract was performed by overpressured layer chromatography (OPLC) with on-line detection, fractionation combined with sample clean-up in-situ in the adsorbent bed after off-line sample application. The antibacterial effect of the eluted fractions and of those compounds remaining on the adsorbent layer after separation was tested with direct bioautography (DB) against the bioluminescent Pseudomonas savastanoi pv. maculicola and Vibrio fischeri. The fractions with high biological activity were analyzed by solid phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) and liquid chromatography and tandem mass spectrometry (LC-MS/MS). Two active uneluted compounds were characterized by off-line OPLC-MS using a thin-layer chromatography (TLC)-MS interface. Mainly, essential oil components, coumarins, flavonoids, phenolic acids, and fatty acids were identified in the active fractions.

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Authors: Krisztián Kovács, Barna Vásárhelyi, Katalin Mészáros, Attila Patócs and Gellért Karvaly

Absztrakt:

Az ösztrogénhormonok fiziológiai szerepe sok tekintetben ismert. Meglehetősen kevés információ áll azonban rendelkezésre az ösztron és az ösztradiol lebontása során képződő vegyületek szerepéről a különböző, ösztrogénhatással összefüggésbe hozott kórképekben. A kutatások intenzív érdeklődésének középpontjában jelenleg a két ösztrogénhormon mellett tizenhárom extragonadális metabolit áll. A képződő metabolitok protektív vagy éppen proinflammatorikus és/vagy proonkogén hatással rendelkeznek. A szisztémás keringésben mért metabolitszintek nem mutatnak összefüggést a lokálisan megjelenő metabolitokéval, ennek a jövőben diagnosztikai jelentősége lehet. A jelen tanulmány célja a perifériás szövetekben az extragonadális metabolommal kapcsolatos irodalmi források átfogó áttekintése, valamint felhívni a figyelmet a perifériás szövetek ösztrogénhomeosztázisának szerepére, az ösztrogénmetabolom igazolt, valamint a klasszikus hormonhatásoktól eltérő biológiai aktivitására, egyes kórfolyamatokban azonosított klinikai jelentőségére. Ezek az ismeretek a lokálisan determinált kórfolyamatok megértését, korai diagnosztikáját a későbbiekben a metabolomika eszköztárával jelentősen segíthetik. Orv Hetil. 2017; 158(24): 929–937.

Open access

An accurate and rapid liquid chromatography–electrospray ionizaion– tandem mass spectrometry (LC—ESI—MS/MS) analytical method was developed and validated for the simultaneous determination of antcins A, B, C, H, and K, dehydroeburicoic acid, and 4,7-dimethoxy-5-methyl-1,3-benzodioxole in the extract and capsule of Antrodia cinnamomea (AC) fruiting body. These seven signature compounds were ionized using an electrospray ion source and analyzed by a triple-quadrupole mass analyzer under a multiple reaction monitoring (MRM) mode. The MRM transitions of m/z 453/409 (antcin A), m/z 467/408 (antcin B), m/z 469/425 (antcin C), m/z 485/413 (antcin H), m/z 487/407 (antcin K), m/z 467/337 (dehydroeburicoic acid), and m/z 197/139 (4,7-dimethoxy-5-methyl-1,3-benzodioxole) were used to quantify these seven components, respectively. Their calibration curves presented good linear regressions (R 2 > 0.997) within the tested concentration range. The intra- and inter-day precisions were less than 1.97% and 2.53%, respectively. The overall recovery was in the range of 87.55%–95.41%. This validated high-performance liquid chromatography (HPLC)—MS/MS method offers promising applications for the accurate and rapid quantification of signature compounds in the fruiting body and its commercial products.

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