Simultaneous determination of wogonin, scutellarin, baicalin and baicalein in the extracts from Scutellariae baicalensis by high performance liquid chromatography with tandem mass spectrometry

T15N1

D.I. Baygildieva, T.M. Baygildiev, A.N. Stavrianidi, O.A. Shpigun, I.A. Rodin

Scutellariae baicalensis is one of the most popular herb in the traditional Chinese medicine. It is used for the treatment of inflammatory process, hypertension, cardiovascular diseases, and also in treatment of bacterial and virus infections due to such active components as wogonin, scutellarin, baicalin and baicalein that are contained in this herb. A sensitive and selective technique of simultaneous determination of these compounds in the extracts from plants raw materials using high performance liquid chromatography tandem mass spectrometry with electrospray ionization was developed. The proposed method has been successfully tested on the commercially available samples of Scutellariae baicalensis root. Analysis of samples was carried out using a reversed-phase chromatography with Acclaim RSLC C18 sorbent. Using multiple reactions monitoring the following limits of detection were achieved: 1 ng mL–1 for wogonin and baicalin, 3 ng mL–1 for scutellarin and 4 ng mL–1 for baicalein. It was found that calibration curve was linear in the concentration range of 20 ng mL–1 and 2000 ng mL–1 for scutellarin and 20 ng mL–1 and 500 ng mL–1 for wogonin, baicalin and baicalein.

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Determination of methylphosphonic acid in human blood plasma by high-performance liquid chromatography tandem mass spectrometry

T13N4

T.M. Baygildiev, I.A. Rodin, A.N. Stavrianidi, A.V. Braun, O.A. Shpigun, I.V. Rybalchenko

 Using high performance liquid chromatography combined with tandem mass spectrometric detection, an approach for the determination of the most stable nerve agent biomarker, methylphosphonic acid, in human blood plasma has been developed. The proposed method is based on the derivatization reaction of methylphosphonic acid with p-bromophenacyl bromide. Optimization of conditions for human plasma sample preparation, mass spectrometric detection conditiones and gradient elution program has been performed. The proposed approach has demonstrated satisfactory reproducibility and selectivity of the determination, limit of detection for methylphosphonic acid in human plasma was 3 ng ml−1.

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Application of high-performance liquid chromatography / high resolution mass spectrometry for investigation of sodium 2,3-disulfanyl- 1-propanesulfonate (unithiol) and products of its oxidation with hydrogen peroxide

T13N2

D.O. Kuleshov, T.E. Berezkina, Y. V. Russkikh, E. N. Chernova, Z. A. Zhakovskaya,
S.V. Masyukevich, L.N. Gall, N.R. Gall

High-performance liquid chromatography combined with high resolution mass spectrometry has been used to study soft oxidation of sodium 2,3-disulfanyl-1-propanesulfonate (unithiol) with hydrogen peroxide; reference peaks were identified for initial substance and reaction products. The possibility to use high-performance liquid chromatography with high resolution mass spectrometry for Sokolovsky thiol-disulphide test has been shown.

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Features of determination of residual amounts of chloramphenicol and tetracycline in food by high performance liquid chromatography/high resolution quadrupole time-of-flight mass spectrometry

T13N2

V.G. Amelin, N.M. Fedina, A.I. Korotkov Читать полностью

High sensitive determination of 1,1-dimethylhydrazine by high-performance liquid chromatography – tandem mass-spectrometry with pre-column derivatization by phenylglyoxal

T12N4

S.V. Osipenko, R.S. Smirnov, A.D. Smolenkov, O.A. Shpigun Читать полностью

Profiling of phytoecdysteroids in extract of sawwort (Serratula coronata) using high-performance liquid chromatography / high resolution tandem mass spectrometry

T12N3

D.A. Sevko, M.K. Beklemishev, I.A. Rodin, A.A. Ihalaynen,
A.M. Antokhin, V.F. Taranchenko, V.M. Goncharov,
D.A. Mitrofanov, A.V. Aksenov

This paper reports the research of phytoecdysteroids in extract of sawwort (Serratula coronatа) by high-performance liquid chromatography coupled with high resolution mass-spectrometry. Mass-spectra of target analytes including tandem mass-spectra are obtained. Fragmentation of phytoecdysteroids negative ions, generated using electrospray ionization, is studied. Structures of target analytes are proposed. Quantitative assessment of identified compounds is carried out.

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Determination of flavonoids of Epimedium by high performance liquid chromatography with tandem mass spectrometric detection

T12N2

O.A. Shevlyakova, K.J. Vasil’yev, A.A. Ihalaynen, A.M. Antokhin,
V.F. Taranchenko, V.M. Goncharov, A.V. Aksenov, D.A. Mitrofanov,
I.A. Rodin, O.A. Shpigun

An approach for simultaneous detection of icariin, icaritin, icarisides I, II, epimedins A, B, C in extracts from plants and сommегсial pгoduсts was developed on the basis of liquid chromatography/mass spectrometry. Using the dry and liquid extracts of Epimedium and the tea, the validation of the approach was carried out. Limits of detection were 5×10−4 mkg ml−1. For compounds determination, electrospray ionization in positive ion mode and tandem mass spectrometric detection in multiple reaction monitoring mode were used.

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Determination of nerve agent hydrolysis products in natural waters by liquid chromatography/mass spectrometry

T12N2

I.A. Rodin, A.V. Braun, T.M. Baygildiev, I.A. Anan’eva, O.A. Shpigun, I.V. Rybalchenko

An approach to the determination of four nerve agents markers – S-(2-diethylaminoethyl) methylphosphonotioate, S-(2-diisopropylaminoethyl) methylphosphonotioate, bis (2-N,N-diethylaminoetil) disulfide and bis(2-N,N-diisopropylaminoethyl) disulfide – in aqueousenvironmental samples with the use of HPLC with tandem mass spectrometric detection was first developed. Optimal mass spectrometric detection and LC separation conditions were developed during the work. The proposed approach was applied to the analysis of real water samples and showed absence of matrix effect, good accuracy, reproducibility and selectivity. Detection limits achieved for S-(2-diethylaminoethyl) methylphosphonotioat, S-(2-diisopropylaminoethyl) methylphosphonotioat, bis(2-N,N-diethylaminoethyl) disulfide, and bis(2-N,N-diisopropylaminoethyl) disulfide in water samples were 0.0003, 0.003, 0.3 and 0.05 mg ml–1, respectively.

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High-resolution time of flight mass spectrometry combined with high performance liquid chromatography for detection and determination of quinolones and sulfonamides in foods

T12N2

V.G. Amelin, A.I. Korotkov, N.M. Volkova

Method of high-resolution time-of-flight mass spectrometry combined with high performance liquid chromatography has been developed for the detection and determination of residues of 23 quinolones (fluoroquinolones) and a number of sulfonamides in foods. The samples were prepared using simplified and quick sample preparation. The limits of detection of quinolones and sulfonamides ranged from 0.05 (1) to 1000 (2000) mkg kg‒1. A scheme for identification and determination of detected quinolones has been developed using method of standard addition. The relative standard deviations of analysis results are less than 0.1.

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Some aspects of experimental design in the targeted proteomics based on using selected reaction monitoring and isotope-labeled peptides

T11N3

Some aspects of experimental design in the targeted proteomics based
on using selected reaction monitoring and isotope-labeled peptides

E.D. Virus, A.V. Ivanov, B.P. Luzyanin, A.A. Kubatiev Читать полностью