Interfaces for capillary LC with ICPMS detection: A comparison of nebulizers/spray chamber configurations

Lokits, Kirk; Limbach, Patrick A.; Caruso, Joseph A.

doi:10.1039/b820121h

Cited by 17 publications

(18 citation statements)

References 29 publications

(44 reference statements)

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“…These results also suggest that a larger oligonucleotide component (i.e., more phosphorus per oligonucleotide component) would be advantageous for ICPMS detection when using the HFIP/TEA mobile phase conditions. The LOD values obtained here (≤ μmol concentration) are comparable to values previously reported for cross-link or heteroconjugate characterization by LC-ESI-MS [16-21], and additional investigation of alternative nebulization sources may improve these LOD values further [32]. …”

Section: Resultssupporting

confidence: 86%

“…Because the separation of biomolecules, such as peptides and oligonucleotides, using RP-HPLC typically requires high concentrations of organic solvent or buffer to elute the sample from the column, care must be taken to reduce the overall volume of LC eluent introduced into the ICP source. Thus, we first examined both peptide-based RP-HPLC conditions, where TFA is present in the mobile phase, and conventional oligonucleotide ion-pairing RP-HPLC conditions, where HFIP and TEA are the major components of the mobile phase, using cap-LC to ensure that the mobile phase conditions amenable to ICP-MS [31, 32] would adequately separate the biomolecules of interest. The acidic mobile phases and solution conditions investigated have been utilized previously with heteroconjugates, such as that used here as a model system, and were not found to affect the integrity of the heteroconjugate [13, 21, 25, 26].…”

Section: Resultsmentioning

confidence: 99%

“…Quantitation of post-translationally modified proteins (phosphoproteins and sulfated proteins) by phosphorus or sulfur monitoring during LC-ICPMS analysis of proteolytic digests is now commonly performed [28-31]. Similarly, LC-ICPMS monitoring of phosphorus or sulfur can also be used for the identification and quantification of oligodeoxynucleotides and phosphorothioate oligonucleotides [32, 33]. …”

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Selective Detection of Peptide-Oligonucleotide Heteroconjugates Utilizing Capillary HPLC-ICPMS

Catron

Caruso

Limbach

2012

J. Am. Soc. Mass Spectrom.

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A method for the selective detection and quantification of peptide:oligonucleotide heteroconjugates, such as those generated by protein:nucleic acid cross-links, using capillary reversed-phase high performance liquid chromatography (cap-RPHPLC) coupled with inductively coupled plasma mass spectrometry detection (ICPMS) is described. The selective detection of phosphorus as 31P+, the only natural isotope, in peptide-oligonucleotide heteroconjugates is enabled by the elemental detection capabilities of the ICPMS. Mobile phase conditions that allow separation of heteroconjugates while maintaining ICPMS compatibility were investigated. We found that trifluoroacetic acid (TFA) mobile phases, used in conventional peptide separations, and hexafluoroisopropanol/triethylamine (HFIP/TEA) mobile phases, used in conventional oligonucleotide separations, both are compatible with ICPMS and enable heteroconjugate separation. The TFA-based separations yielded limits of detection (LOD) of ~40 ppb phosphorus, which is nearly seven times lower than the LOD for HFIP/TEA-based separations. Using the TFA mobile phase, 1-2 pmol of a model heteroconjugate were routinely separated and detected by this optimized capLC-ICPMS method.

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Section: Resultssupporting

confidence: 86%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Selective Detection of Peptide-Oligonucleotide Heteroconjugates Utilizing Capillary HPLC-ICPMS

Catron

Caruso

Limbach

2012

J. Am. Soc. Mass Spectrom.

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“…Aside from these problems that are mainly related to the plasma solvent load, coupling HPLC-based methods with ICP-MS detection is a relatively straightforward task, as the eluent flow of the separation module is within the sample uptake range of these systems, or can at least be matched by either selecting the flow rate (by selecting a standard, micro-, or nanobore HPLC system) [35] or adapting the nebulizing system (standard-, micro-, or nanoflow nebulizer) [36].…”

Section: Hplc/icp-msmentioning

confidence: 99%

Hyphenated techniques as tools for speciation analysis of metal-based pharmaceuticals: developments and applications

Meermann

Sperling

2012

Anal Bioanal Chem

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Method development and applications of hyphenated techniques as tools for speciation analysis of metal-based pharmaceuticals are summarized within this review. Advantages and limitations of the separation modes-high-performance liquid chromatography (HPLC), capillary electrophoresis (CE), and gas chromatography (GC)-as well as the detection modes-inductively coupled plasma-mass spectrometry (ICP-MS) and electrospray ionization-mass spectrometry (ESI-MS)-are discussed. ICP-MS detection is found to be advantageous for the quantification of drugs containing metals and other heteroatoms. The species-independent sensitivity and multielement capabilities of ICP-MS allow it to be used for quantification even when species-specific standards are not available, as well as to determine the stoichiometry in metallodrug-biomolecule interactions. Molecular information that is totally destroyed when ICP is applied as ionization source and is therefore not obtainable via ICP-MS detection can be accessed by the complementary technique of ESI-MS. Speciation analysis combining both elemental and molecular information is therefore a powerful tool for the analysis of metal-based pharmaceuticals and their metabolites in body fluids and other relevant matrices.

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“…coupling. Particular attention must be paid both to the quality of the aerosol produced through the nebulizer/spray chamber [50] and to the contribution of the whole interface to peak band broadening [3,44,45,[51][52][53], both features being able to significantly affect the sensitivity. A well-documented summary of SIS devices was reported by Leclerq and al.…”

Section: Lc-icp-ms Interfacementioning

confidence: 99%

Suitable interface for coupling liquid chromatography to inductively coupled plasma-mass spectrometry for the analysis of organic matrices. 1 Theoretical and experimental considerations on solute dispersion

Bernardin

Bessueille-Barbier

Masle

et al. 2018

Journal of Chromatography A

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Liquid chromatography (LC) hyphenated to a specific detection such as inductively coupled plasma-mass spectrometry (ICP-MS) is a technique of choice for elemental speciation analysis. However, various instrumental limitations may considerably reduce the expected sensitivity of the technique. Among those, we were interested by the solute dispersion into the interface located between LC and ICP-MS. The interface consists of a Sample Introduction System (SIS) and a possible flow-splitter prior to SIS. Flow splitting can be required in case of organic matrices to reduce the organic solvent amount entering plasma which may lead to plasma instabilities. Although extra-column dispersion is usually well taken into account with conventional UV detection it has been little studied in the context of LC-ICP-MS and moreover never quantified. Our objective is to assess the loss in column plates and hence in both separation quality and sensitivity which may be generated by the coupling of LC and ICP-MS in the specific case of organic matrices. In this first study, this is done (1) from a theoretical approach; (2) from 55 experimental studies reported in LC-ICP-MS and (3) from our experimental results highlighting the critical impact of the flow splitter on extra-column dispersion depending on both flow-rate and split ratio. It turns out by evaluating the 55 reported studies by means of theoretical calculations, that the loss in plates due to extra-column dispersion was most of the time beyond 50% and even often beyond 90%. Moreover, from our experiments, it has been shown that a very low split ratio (1:50) could generate an additional variance around 200 μL² which induces a loss in theoretical plate of 90% for ultra-high performance LC (UHPLC) column (5 cm × 2.1 mm, 1.7 μm).

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Interfaces for capillary LC with ICPMS detection: A comparison of nebulizers/spray chamber configurations

Cited by 17 publications

References 29 publications

Selective Detection of Peptide-Oligonucleotide Heteroconjugates Utilizing Capillary HPLC-ICPMS

Selective Detection of Peptide-Oligonucleotide Heteroconjugates Utilizing Capillary HPLC-ICPMS

Hyphenated techniques as tools for speciation analysis of metal-based pharmaceuticals: developments and applications

Suitable interface for coupling liquid chromatography to inductively coupled plasma-mass spectrometry for the analysis of organic matrices. 1 Theoretical and experimental considerations on solute dispersion

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