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Rapid communications in mass spectrometry : RCM2023; 37(14); e9530; doi: 10.1002/rcm.9530

Electrospray ionization mass spectrometry adduct formation by mobile phase additives: A case study using nitrile functional groups containing selective androgen receptor modulators.

Abstract: The formation of mass adducts is common during electrospray ionization mass spectrometry (ESI-MS). However, the mechanism that leads to adduct formation is poorly understood and difficult to control. Multiplication of mass adducts at once will adversely impact the sensitivity of mass analysis and cause misinterpretation of the level of detection. Prior studies on selective androgen receptor modulators (SARMs) revealed an immense mass adduct formation in both positive and negative ESI modes. Methods: In this study, additives in the mobile phases are investigated as a potential means of controlling mass adduct formation in various SARMs. Results: The first evidence of chloride adduct formation when SARMs are detected via ESI-MS has been reported in this research. A series of mobile phase combinations were tested to achieve the optimal condition for HPLC-MS. A comparison was also made between adduct formation on various grades of water used for preparing the mobile phase. A validation study using equine urine and plasma was also conducted to assess the suitability of the developed method. Conclusions: The results of this study will allow for a more accurate identification of SARMs, which will make it easier to investigate their illicit use in horse racing.
© 2023 John Wiley & Sons Ltd.
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Publication Date: 2023-05-01 PubMed ID: 37125537DOI: 10.1002/rcm.9530Google Scholar: Lookup
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Summary

This research summary has been generated with artificial intelligence and may contain errors and omissions. Refer to the original study to confirm details provided. Submit correction.

This research paper focuses on the understanding and control of mass adduct formation during electrospray ionization mass spectrometry (ESI-MS), a phenomenon that can negatively impact analysis results. The study further examines the effect of additives in the mobile phases on adduct formation in selective androgen receptor modulators (SARMs) and presents a method to more accurately identify such compounds, which can find use in investigations into illegal horse racing activities.

Understanding Mass Adduct Formation

  • During the process of electrospray ionization mass spectrometry (ESI-MS), mass adducts – complex molecules resulting from the union of two or more simpler ones – often form. This is a common occurrence, yet its mechanism is not fully understood and poses challenges in control.
  • The multiplicity of mass adducts being formed simultaneously does affect the sensitivity of the mass analysis carried out, posing difficulties in detecting and interpreting results.
  • Particular interest in this study was directed at selective androgen receptor modulators or SARMs, a class of drugs with effects similar to anabolic steroids. Past studies have shown significant mass adduct formation involving these compounds, with ESI-MS used in both positive and negative modes.

Role of Mobile Phase Additives

  • Mobile phases, the liquid solution used in chromatographic techniques to carry the sample through the system, often include additives which can interact with the compounds of interest.
  • This study explored these additives as potential factors that might influence mass adduct formation in SARMs.
  • The research also provided the first-ever evidence of chloride adduct formation when SARMs are analyzed through ESI-MS.

Optimization and Validation

  • A series of mobile phase combinations was tested in order to arrive at the optimal conditions for High Performance Liquid Chromatography-Mass Spectrometry (HPLC-MS), a widely-used technique in analytical chemistry.
  • A comparison among different grades of water, used in preparation of mobile phases, was made to evaluate the effect on adduct formation.
  • A practical application of the developed methodology was tested through a validation study on equine urine and plasma samples. This is notably relevant as SARMs are occasionally used illicitly in horse racing to enhance performance.

Conclusion

  • The findings of this research could enhance the accuracy of identifying SARMs, thereby facilitating investigations into illegal use in horse racing.

Cite This Article

APA
Karatt TK, Muhammed Ajeebsanu M, Karakka Kal AK, Subhahar MB, Sathiq MA, Laya S. (2023). Electrospray ionization mass spectrometry adduct formation by mobile phase additives: A case study using nitrile functional groups containing selective androgen receptor modulators. Rapid Commun Mass Spectrom, 37(14), e9530. https://doi.org/10.1002/rcm.9530

Publication

Rapid communications in mass spectrometry : RCM
ISSN: 1097-0231
NlmUniqueID: 8802365
Country: England
Language: English
Volume: 37
Issue: 14
Pages: e9530

Researcher Affiliations

Karatt, Tajudheen Kunhamu
  • Equine Forensic Unit, Central Veterinary Research Laboratory, Dubai, United Arab Emirates.
  • Post Graduate and Research Department of Chemistry, Jamal Mohamed College (Affiliated to Bharathidasan University), Tiruchirappalli, India.
Muhammed Ajeebsanu, Meleparappil
  • Equine Forensic Unit, Central Veterinary Research Laboratory, Dubai, United Arab Emirates.
Karakka Kal, Abdul Khader
  • Equine Forensic Unit, Central Veterinary Research Laboratory, Dubai, United Arab Emirates.
Subhahar, Michael Benedict
  • Equine Forensic Unit, Central Veterinary Research Laboratory, Dubai, United Arab Emirates.
Sathiq, Mohamedkhani Anwar
  • Post Graduate and Research Department of Chemistry, Jamal Mohamed College (Affiliated to Bharathidasan University), Tiruchirappalli, India.
Laya, Saraswathy
  • Department of Chemistry, College of Science, United Arab Emirates University, Al Ain, United Arab Emirates.

MeSH Terms

  • Animals
  • Horses
  • Spectrometry, Mass, Electrospray Ionization / methods
  • Receptors, Androgen
  • Chromatography, High Pressure Liquid / methods
  • Indicators and Reagents
  • Androgens

Grant Funding

  • DST-FIST Funded PG
  • Research Department of Chemistry and the management committee of Jamal Mohamed College, Tiruchirapalli 620020

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