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Determination of IGF-1 and IGF-2, their degradation products and synthetic analogues in urine by LC-MS/MS.
- Source :
-
The Analyst [Analyst] 2011 Mar 07; Vol. 136 (5), pp. 1003-12. Date of Electronic Publication: 2010 Dec 15. - Publication Year :
- 2011
-
Abstract
- Peptide analysis in doping controls by means of nano-UPLC coupled high resolution/high mass accuracy mass spectrometry provides the state-of-the-art technique in modern sports drug testing. The present study describes a recent application of this technique for the qualitative determination of different urinary insulin-like growth factor (IGF) related peptides. After simultaneous isolation by solid phase extraction and magnetic particle-based immunoaffinity purification, target analytes (IGF-1, IGF-2, Des1-3-IGF-1, R(3)-IGF-1 and longR(3)-IGF-1) were separated by nano-liquid chromatography prior to mass spectrometric detection. Endogenously produced IGF-1 and IGF-2, as well as the degradation product Des1-3-IGF-1, were frequently detected in urine samples from healthy volunteers in a concentration range of 20-400 pg mL(-1). The impact of IGF binding proteins (IGFBPs), being also present in urine, was potentially estimated by an additional ultrafiltration step in the sample preparation procedure. The synthetic analogue longR(3)-IGF-1, which is assumed to be subject to misuse by cheating athletes, was also analysed and detected in fortified urine samples. Besides the intact molecule, an N-terminally truncated degradation product Des1-10-longR(3)-IGF-1 was identified as the more stable target for doping controls using urine samples. The method was validated for qualitative purposes considering the parameters specificity, limit of detection (20-50 pg mL(-1)), recovery (10-35%), precision (<20%), linearity, robustness and stability.
- Subjects :
- Doping in Sports
Female
Humans
Limit of Detection
Male
Reproducibility of Results
Solid Phase Extraction methods
Time Factors
Ultrafiltration methods
Chromatography, Liquid methods
Insulin-Like Growth Factor I urine
Insulin-Like Growth Factor II urine
Substance Abuse Detection methods
Tandem Mass Spectrometry methods
Subjects
Details
- Language :
- English
- ISSN :
- 1364-5528
- Volume :
- 136
- Issue :
- 5
- Database :
- MEDLINE
- Journal :
- The Analyst
- Publication Type :
- Academic Journal
- Accession number :
- 21157622
- Full Text :
- https://doi.org/10.1039/c0an00632g