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DMSO assisted electrospray ionization for the detection of small peptide hormones in urine by dilute-and-shoot-liquid-chromatography-high resolution mass spectrometry

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Abstract
The mobile phase additive (DMSO) has been described as a useful tool to enhance electrospray ionization (ESI) of peptides and proteins. So far, this technique has mainly been used in proteomic/peptide research, and its applicability in a routine clinical laboratory setting (i.e., doping control analysis) has not been described yet. This work provides a simple, easy to implement screening method for the detection of doping relevant small peptides (GHRPs, GnRHs, GHS, and vasopressin-analogues) with molecular weight less than 2 kDa applying DMSO in the mobile phase. The gain in sensitivity was sufficient to inject the urine samples after a 2-fold dilution step omitting a time consuming sample preparation. The employed analytical procedure was validated for the qualitative determination of 36 compounds, including 13 metabolites. The detection limits (LODs) ranged between 50 and 1000 pg/mL and were compliant with the 2 ng/mL minimum detection level required by the World Anti-Doping Agency (WADA) for all the target peptides. To demonstrate the feasibility of the work, urine samples obtained from patients who have been treated with desmopressin or leuprolide and urine samples that have been declared as adverse analytical findings were analyzed.
Keywords
Peptides, High-resolution mass spectrometry, Doping control, HRMS, Urine, Dilute-and-shoot, DMSO, DOPING CONTROL ANALYSIS, SOLID-PHASE EXTRACTION, MOBILE-PHASE, EQUINE, IDENTIFICATION, PLASMA, TB-500, SCREEN, MS/MS

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Chicago
Judák, Péter, Janelle Grainger, Catrin Goebel, Peter Van Eenoo, and Koen Deventer. 2017. “DMSO Assisted Electrospray Ionization for the Detection of Small Peptide Hormones in Urine by Dilute-and-shoot-liquid-chromatography-high Resolution Mass Spectrometry.” Journal of the American Society for Mass Spectrometry 28 (8): 1657–1665.
APA
Judák, P., Grainger, J., Goebel, C., Van Eenoo, P., & Deventer, K. (2017). DMSO assisted electrospray ionization for the detection of small peptide hormones in urine by dilute-and-shoot-liquid-chromatography-high resolution mass spectrometry. JOURNAL OF THE AMERICAN SOCIETY FOR MASS SPECTROMETRY, 28(8), 1657–1665.
Vancouver
1.
Judák P, Grainger J, Goebel C, Van Eenoo P, Deventer K. DMSO assisted electrospray ionization for the detection of small peptide hormones in urine by dilute-and-shoot-liquid-chromatography-high resolution mass spectrometry. JOURNAL OF THE AMERICAN SOCIETY FOR MASS SPECTROMETRY. 2017;28(8):1657–65.
MLA
Judák, Péter, Janelle Grainger, Catrin Goebel, et al. “DMSO Assisted Electrospray Ionization for the Detection of Small Peptide Hormones in Urine by Dilute-and-shoot-liquid-chromatography-high Resolution Mass Spectrometry.” JOURNAL OF THE AMERICAN SOCIETY FOR MASS SPECTROMETRY 28.8 (2017): 1657–1665. Print.
@article{8544538,
  abstract     = {The mobile phase additive (DMSO) has been described as a useful tool to enhance electrospray ionization (ESI) of peptides and proteins. So far, this technique has mainly been used in proteomic/peptide research, and its applicability in a routine clinical laboratory setting (i.e., doping control analysis) has not been described yet. This work provides a simple, easy to implement screening method for the detection of doping relevant small peptides (GHRPs, GnRHs, GHS, and vasopressin-analogues) with molecular weight less than 2 kDa applying DMSO in the mobile phase. The gain in sensitivity was sufficient to inject the urine samples after a 2-fold dilution step omitting a time consuming sample preparation. The employed analytical procedure was validated for the qualitative determination of 36 compounds, including 13 metabolites. The detection limits (LODs) ranged between 50 and 1000 pg/mL and were compliant with the 2 ng/mL minimum detection level required by the World Anti-Doping Agency (WADA) for all the target peptides. To demonstrate the feasibility of the work, urine samples obtained from patients who have been treated with desmopressin or leuprolide and urine samples that have been declared as adverse analytical findings were analyzed.},
  author       = {Jud{\'a}k, P{\'e}ter and Grainger, Janelle and Goebel, Catrin and Van Eenoo, Peter and Deventer, Koen},
  issn         = {1044-0305},
  journal      = {JOURNAL OF THE AMERICAN SOCIETY FOR MASS SPECTROMETRY},
  keyword      = {Peptides,High-resolution mass spectrometry,Doping control,HRMS,Urine,Dilute-and-shoot,DMSO,DOPING CONTROL ANALYSIS,SOLID-PHASE EXTRACTION,MOBILE-PHASE,EQUINE,IDENTIFICATION,PLASMA,TB-500,SCREEN,MS/MS},
  language     = {eng},
  number       = {8},
  pages        = {1657--1665},
  title        = {DMSO assisted electrospray ionization for the detection of small peptide hormones in urine by dilute-and-shoot-liquid-chromatography-high resolution mass spectrometry},
  url          = {http://dx.doi.org/10.1007/s13361-017-1670-7},
  volume       = {28},
  year         = {2017},
}

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