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[Simultaneous identification and detection of 16 anabolic steroid hormones in muscle using liquid chromatography oupled to quadrupole/linear ion trap mass spectrometry].
- Source :
-
Se pu = Chinese journal of chromatography [Se Pu] 2012 Oct; Vol. 30 (10), pp. 991-1001. - Publication Year :
- 2012
-
Abstract
- A comprehensive method for simultaneous identification and detection of 16 anabolic steroid hormones (ASs, including andorgens, gestagens and their esters) in muscle samples was developed with liquid chromatography coupled to quadrupole/linear ion trap mass spectrometry (LC-Q/Trap-MS). The ASs in muscle samples were extracted with acetonitrile under ultrasonic assistance. The extract was defatted by n-hexane with liquid-liquid partitioning and followed by clean-up with NH2 solid phase extraction (SPE) cartridge. The separation of analytes was carried out on a CAPCELL PAK C18 MG II column (150 mm x 2.0 mm, 5.0 microm) using mobile phases of 0.1% (v/v) formic acid in acetonitrile and 0.1% (v/v) formic acid-5 mmol/L ammonium formate aqueous solution with gradient elution. A scheduled multiple reaction monitoring (sMRM) in positive mode as survey scan and an enhanced product ion (EPI) scan as dependent scan in an information-dependent acquisition (IDA) experiment was adopted in mass spectrometry acquisition. On-line lab-built MS/MS library and internal standards were employed for the identification and quantification. As a result, the 16 ASs showed good linearity with all correlation coefficients (r) no less than 0. 999 0 within the linear ranges. The limits of quantification (LOQs, S/N > or = 10) for the 16 ASs were in the range of 0.029-0.36 microg/kg. At the three spiked levels (0.5, 2.0 and 20 microg/kg), the overall recoveries ranged from 89.9% to 118% with the relative standard deviations (RSDs) no more than 16.2% under within--laboratory reproducibility conditions. The proposed method can be used to identify and detect the 16 ASs in a single run, which makes it effective in residue surveillance of anabolic hormones in muscle samples.
Details
- Language :
- Chinese
- ISSN :
- 1000-8713
- Volume :
- 30
- Issue :
- 10
- Database :
- MEDLINE
- Journal :
- Se pu = Chinese journal of chromatography
- Publication Type :
- Academic Journal
- Accession number :
- 23383485
- Full Text :
- https://doi.org/10.3724/sp.j.1123.2012.08017