High-performance liquid chromatography integrated solid-phase extraction in bioanalysis using restricted access precolumn packings

Boos, Karl-Siegfried

doi:10.1016/s0165-9936(98)00102-2

Cited by 147 publications

(71 citation statements)

References 25 publications

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“…The further eliminations of H 2 O and NH 3 ϩ· ), with the latter being the most abundant. From these two product ions multiple losses of HCN and/or CO showed, as commonly seen in the dissociation pathways of nucleosides [5,6,9,15,16]. It has to be noted that once more an addition of H 2 O in the collision cell was observed; the radical ion at m/z 109 formed an adduct with H 2 O yielding the radical ion at m/z 127 (C 4 …”

Section: : a Results Of Ch 3 Oh-adduct Formation And Ch 3 Oh-gas-phasementioning

confidence: 84%

In-source CID of guanosine: Gas phase ion-molecule reactions

Tuytten

Lemière

Esmans

et al. 2006

J. Am. Soc. Mass Spectrom.

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In-source collision induced dissociation was applied to access second generation ions of protonated guanosine. The in-source gas-phase behavior of [BH 2 ] ϩ -NH 3 (m/z 135, C 5 H 3 N 4 O ϩ ) was investigated. Adduct formation and reactions with available solvent molecules (H 2 O and CH 3 OH) were demonstrated. Several addition/elimination sequences were observed for this particular ion and solvent molecules. Dissociation pathways for the newly formed ions were developed using a QqTOF mass spectrometer, permitting the assignment of elemental compositions of all product ions produced. Reaction schemes were suggested arising from the ring-opened intermediate of the protonated base moiety [BH 2 ] ϩ , obtained from fragmentation of guanosine. The mass spectral data revealed that the in-source CH 3 OH-reaction product underwent more complex fragmentations than the comparable ion following reaction with H 2 O. A rearrangement and a parallel radical dissociation pathway were discerned. Apart from the mass spectrometric evidence, the fragmentation schemes are supported by density functional theory calculations, in which the reaction of the ring-opened protonated guanine intermediate with CH 3 OH and a number of subsequent fragmentations were elaborated. uring the last decade, most fragmentation pathways were elaborated on triple quadrupole (QqQ) and particularly quadrupole ion-trap (QIT) instruments. The latter's capabilities of accessing MS n product ions by applying repeated stages of mass selection and fragmentation proved to be very useful [1]. The maturation of the time of flight (TOF) technology and, more importantly, its use in hybrid-arrangements such as the popular orthogonal QqTOF mass spectrometer made accurate mass data of product ions more readily available [2]. In many cases, the elemental compositions of the product ions can unambiguously be assigned when using a QqTOF mass spectrometer. Product ions lower in the genealogical ladder are also accessible by applying relatively high collision energies in the collision cell. Yet disentanglement of different dissociation pathways originating from a communal progenitor is -in general-still confined to QIT set ups, although the interpretation of energy resolved spectra also has proven its usefulness [3].Recently we and others showed [4 -6] that by making optimal use of in-source CID, combined with the inherent tandem MS capabilities of the QqTOF, what is in effect up to MS 5 data can be acquired. Compared to QIT data the QqTOF data obtained is superior in respect of higher mass accuracy. On the other hand QIT-CID experiments, in general, access almost exclusively the dissociation reaction channels of the lowest energy of activation [7]. This energy-dependent information can

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Section: : a Results Of Ch 3 Oh-adduct Formation And Ch 3 Oh-gas-phasementioning

confidence: 84%

In-source CID of guanosine: Gas phase ion-molecule reactions

Tuytten

Lemière

Esmans

et al. 2006

J. Am. Soc. Mass Spectrom.

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“…(Souverain et al, 2004). A RAM support developed by Boos and Grimm (Boos & Grimm, 1999) is based on SCX-diol modification to improve performances in terms of efficiency, retention and reproducibility. Račaitytė et al (Račaitytė et al 2000) have shown that this type of RAMs is highly suitable for the on-line extraction and analysis of neuropeptides in plasma.…”

Section: Restricted Access Materials Columnsmentioning

confidence: 99%

Profiling of Endogenous Peptides by Multidimensional Liquid Chromatography

Machtejevienė¹,

Machtejevas²

2012

Biomarker

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“…Among the restricted access sorbents, a family belonging to the group of internal surface reversed-phase (ISRP) supports, namely alkyl diol silica (ADS), packed in pre-columns has been applied successfully for the clean-up of plasma samples prior to LC analysis [6][7][8][9][10][11][12][13][14]. The topochemistry of the ADS sorbents has been represented schematically elsewhere [6,8,13,15,16]. Due to the appropriate pore diameter (about 6 nm) of the silica particles, macromolecules, such as proteins, having a molecular mass larger than 15 kDa, are excluded in the void volume of the pre-column and are directly flushed into the waste.…”

Section: Introductionmentioning

confidence: 99%

Automated method for the determination of a new matrix metalloproteinase inhibitor in ovine plasma and serum by coupling of restricted access material for on-line sample clean-up to liquid chromatography

Chiap

Piette

Évrard

et al. 2005

Journal of Chromatography B

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A fully automated liquid chromatographic method was developed for the determination of Ro 28-2653, a new synthetic inhibitor of matrix metalloproteinase s (MMPs), in ovine serum and plasma. The method was based on the coupling of a pre-column packed with restricted access material, namely LiChrospher RP-8 ADS (alkyl diol silica), for sample clean-up to an analytical column containing octyl silica stationary phase. One hundred µl of biological sample, to which 2-propanol was automatically added, were injected onto the ADS pre-column, which was then washed with a washing liquid consisting of a mixture of 25 mM phosphate buffer (pH 7.0) and acetonitrile (90:10; v/v) for 10 min. By rotation of the switching valve, the analyte was then eluted in the backflush mode with the LC mobile phase composed of a mixture of acetonitrile and 25 mM phosphate buffer (pH 7.0) (57:43; v/v). The UV detection was performed at 395 nm. The main parameters likely to influence the sample preparation technique were investigated. The method was then validated over a concentration range from 17.5 to 1950 ng/ml, the first concentration level corresponding to the lower limit of quantitation. At this concentration level, the mean bias and the R.S.D. value for intermediate precision were -2.4% and 4.2%, respectively.

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High-performance liquid chromatography integrated solid-phase extraction in bioanalysis using restricted access precolumn packings

Cited by 147 publications

References 25 publications

In-source CID of guanosine: Gas phase ion-molecule reactions

In-source CID of guanosine: Gas phase ion-molecule reactions

Profiling of Endogenous Peptides by Multidimensional Liquid Chromatography

Automated method for the determination of a new matrix metalloproteinase inhibitor in ovine plasma and serum by coupling of restricted access material for on-line sample clean-up to liquid chromatography

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