Atmospheric Pressure Ionization Using a High Voltage Target Compared to Electrospray Ionization

Lubin, Arnaud; Bajic, Steve; Cabooter, Deirdre; Augustijns, Patrick; Cuyckens, Filip

doi:10.1007/s13361-016-1537-3

Cited by 18 publications

(29 citation statements)

References 32 publications

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“…Acetonitrile of analytical grade, dimethyl sulfoxide (DMSO) (for HPLC, >99.7%) and formic acid were purchased from Merck (Darmstadt, Germany). All MOTS-c peptides including human (h), mouse (m), human (1)(2)(3)(4)(5)(6)(7)(8)(9)(10)(11)(12)(13) , human (1)(2)(3)(4)(5)(6)(7)(8)(9)(10)(11)(12) and rat (1)(2)(3)(4)(5)(6)(7)(8)(9)(10)(11)(12)(13)(14) analogues (purity ≥95%) were obtained from Phoenix Pharmaceuticals, Inc. (Burlingame, CA, USA). As internal standard (ISTD), six-fold 13 Tris-(2-carboxyethyl)phosphine hydrochloride (≥98%, TCEP) was from Carl Roth GmbH + Co. KG (Karlsruhe, Germany).…”

Section: Chemicals and Materialsmentioning

confidence: 99%

“…The reconstituted analytes were analyzed by means of high‐performance liquid chromatography coupled via UniSpray™ (US) ionization to triple quadrupole tandem mass spectrometry. US represents a new atmospheric pressure ionization (API) technique which is attributed to improved intensity gain (sensitivity) in comparison with ESI sources and reduced matrix effects for plasma samples . Supplementing the analytical capacity, animal variants as well as truncated derivatives, which are commercially available, were characterized by high‐resolution mass spectrometry (HRMS).…”

Section: Introductionmentioning

confidence: 99%

“…US represents a new atmospheric pressure ionization (API) technique which is attributed to improved intensity gain (sensitivity) in comparison with ESI sources and reduced matrix effects for plasma samples. 9,10 Supplementing the analytical capacity, animal variants as well as truncated derivatives, which are commercially available, were characterized by high-resolution mass spectrometry (HRMS). In vitro metabolic studies and stability tests were conducted to identify potential metabolic degradation and oxidation products.…”

Section: Introductionmentioning

confidence: 99%

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Development of a mass spectrometry based detection method for the mitochondrion‐derived peptide MOTS‐c in plasma samples for doping control purposes

Knoop

Thomas

Thevis

2019

Rapid Comm Mass Spectrometry

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Rationale The mitochondrial open reading frame of 12S rRNA type‐c (MOTS‐c) peptide was recently discovered and described to control metabolic homeostasis through AMPK activation along with AICAR accumulation. Consequently, it appears advisable to monitor the potential use of synthetic MOTS‐c in sports, and a detection method suitable for sports drug testing purposes is necessary. Methods For the detection of MOTS‐c in doping control plasma samples, a test method employing liquid chromatography and mass spectrometry (LC/MS) was developed. Following optimization, the assay was comprehensively validated and additional parameters such as the (long‐term) stability and in vitro metabolism of the peptide were evaluated. In order to determine endogenous MOTS‐c reference limits, the results generated by LC/MS‐based detection were compared with those obtained with a commercially available enzyme‐linked immunosorbent assay (ELISA). Results The LC/MS‐based test method was fully validated for quantitative results interpretation according to the World Anti‐Doping Agency's International Standard for Laboratories (WADA's ISL). It was found to be specific and sensitive, enabling a lower limit of detection (LLOD) for hMOTS‐c in plasma at 100 pg/mL. Following optimization, animal MOTS‐c analogues and four metabolites as well as two oxidation products were implemented. However, endogenous levels of a reference population of 20 healthy subjects studied by ELISA experiments (45.9–218.5 ng/mL) could not be confirmed by LC/MS. Conclusions A mass spectrometric detection assay for MOTS‐c in human plasma samples was developed and successfully validated according to WADA's ISL, providing an additional tool for future doping control purposes. Besides MOTS‐c, the assay also includes four in vitro derived metabolites and two oxidation products, which might further improve the traceability of the drug. The analytical approach was compared with a commercially available ELISA, and considerable differences in measured MOTS‐c levels were observed.

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Section: Chemicals and Materialsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Development of a mass spectrometry based detection method for the mitochondrion‐derived peptide MOTS‐c in plasma samples for doping control purposes

Knoop

Thomas

Thevis

2019

Rapid Comm Mass Spectrometry

View full text Add to dashboard Cite

show abstract

“…Each manufacturer of MS equipment has its own flavor of ESI and APCI source; some have specific sources that are advantageous for specific analytes (eg, APPI) or for specific applications (eg, desorption electrospray ionization (DESI) of Direct Analysis in Real Time (DART) for ionization of analytes on a surface . New ionization methods and sources are developed as well, such as UniSpray™ that extend the range of analytes that can be ionized and analyzed with MS.…”

Section: Conclusion and Future Perspectivesmentioning

confidence: 99%

A tutorial in small molecule identification via electrospray ionization‐mass spectrometry: The practical art of structural elucidation

Vijlder

Valkenborg

Lemière

et al. 2017

Mass Spectrometry Reviews

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178

134

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The identification of unknown molecules has been one of the cornerstone applications of mass spectrometry for decades. This tutorial reviews the basics of the interpretation of electrospray ionization‐based MS and MS/MS spectra in order to identify small‐molecule analytes (typically below 2000 Da). Most of what is discussed in this tutorial also applies to other atmospheric pressure ionization methods like atmospheric pressure chemical/photoionization. We focus primarily on the fundamental steps of MS‐based structural elucidation of individual unknown compounds, rather than describing strategies for large‐scale identification in complex samples. We critically discuss topics like the detection of protonated and deprotonated ions ([M + H]+ and [M − H]−) as well as other adduct ions, the determination of the molecular formula, and provide some basic rules on the interpretation of product ion spectra. Our tutorial focuses primarily on the fundamental steps of MS‐based structural elucidation of individual unknown compounds (eg, contaminants in chemical production, pharmacological alteration of drugs), rather than describing strategies for large‐scale identification in complex samples. This tutorial also discusses strategies to obtain useful orthogonal information (UV/Vis, H/D exchange, chemical derivatization, etc) and offers an overview of the different informatics tools and approaches that can be used for structural elucidation of small molecules. It is primarily intended for beginning mass spectrometrists and researchers from other mass spectrometry sub‐disciplines that want to get acquainted with structural elucidation are interested in some practical tips and tricks.

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“…Finally, as the droplets grow smaller and smaller, ions get released in to gaseous phase by a mechanism called rayleigh scattering/columbic explosion. The emitted ions are sampled by a sampling skimmer cone and are then accelerated into the mass analyzer for subsequent measurement of molecular mass and ion intensity [21][22][23][24]. An important characteristic of ESI-MS is it works as a concentration-dependent detector, which means MS response is directly proportional to concentration of analyte.…”

Section: Electrospray Ionization (Esi)mentioning

confidence: 99%

Mass Spectrometry as a Workhorse for Preclinical Drug Discovery: Special Emphasis on Drug Metabolism and Pharmacokinetics

Veeravalli¹,

Madgula²,

Srivastava³

2019

Mass Spectrometry - Future Perceptions and Applications

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Mass spectrometry as an instrument is popular, given its sensitivity, selectivity, speed and robustness. In this chapter, we have briefly deliberated on various mass spec platforms, their hardware components and specific applications in preclinical drug discovery with a special emphasis on drug metabolism and pharmacokinetic assays. Basic principle of operation of mass spectrometer and various ionization techniques/mass analyzers was explicitly discussed. Compatibility of mass spectrometers with ultrafast LC and various throughput techniques, enabled evaluation of thousands of compounds with quick turnaround times. Faster generation of results corresponding to in vitro ADME and in vivo pharmacokinetic assays, aid medicinal chemists to refine their combinatorial synthetic chemistry efforts and expedite the lead optimization and identification phases of drug discovery. Mass spectrometer is a powerful tool for both qualitative and quantitative applications. While quantitative applications include measurement of absolute/relative concentrations, qualitative features assist in identification of molecular structures of metabolites and putative biotransformation pathways. Qualitative inputs are more precise and accurate, with the advent of high-resolution mass spectrometry technology. Although, mass spectrometry has many built-in advantages, it also suffers from matrix effects, as the samples analyzed are mostly of biological origin and are complex in nature. In this chapter, we have defined the nature of matrix effects and various approaches by which these matrix effects can be mitigated.

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Atmospheric Pressure Ionization Using a High Voltage Target Compared to Electrospray Ionization

Cited by 18 publications

References 32 publications

Development of a mass spectrometry based detection method for the mitochondrion‐derived peptide MOTS‐c in plasma samples for doping control purposes

Development of a mass spectrometry based detection method for the mitochondrion‐derived peptide MOTS‐c in plasma samples for doping control purposes

A tutorial in small molecule identification via electrospray ionization‐mass spectrometry: The practical art of structural elucidation

Mass Spectrometry as a Workhorse for Preclinical Drug Discovery: Special Emphasis on Drug Metabolism and Pharmacokinetics

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