## Abstract An HPLC non‐aqueous reversed‐phase separation system was adapted for analyzing insect triacylglycerols (TAG). The method uses two conventional Nova‐Pak C18 columns connected in series, for a total length of 45 cm. The mobile phase gradient is mixed from acetonitrile and 2‐propanol, and
Liquid chromatography/mass spectrometry in anabolic steroid analysis—optimization and comparison of three ionization techniques: electrospray ionization, atmospheric pressure chemical ionization and atmospheric pressure photoionization
✍ Scribed by Antti Leinonen; Tiia Kuuranne; Risto Kostiainen
- Publisher
- John Wiley and Sons
- Year
- 2002
- Tongue
- English
- Weight
- 119 KB
- Volume
- 37
- Category
- Article
- ISSN
- 1076-5174
- DOI
- 10.1002/jms.328
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✦ Synopsis
Abstract
The applicability of liquid chromatography/tandem mass spectrometry (LC/MS/MS) for the detection of the free anabolic steroid fraction in human urine was examined. Electrospray ionization (ESI), atmospheric pressure chemical ionization and atmospheric pressure photoionization methods were optimized regarding eluent composition, ion source parameters and fragmentation. The methods were compared with respect to specificity and detection limit. Although all methods proved suitable, LC/ESI‐MS/MS with a methanol–water gradient including 5 mM ammonium acetate and 0.01% acetic acid was found best for the purpose. Multiple reaction monitoring allowed the determination of steroids in urine at low nanogram per milliliter levels. LC/MS/MS exhibited high sensitivity and specificity for the detection of free steroids and may be a suitable technique for screening for the abuse of anabolic steroids in sports. Copyright © 2002 John Wiley & Sons, Ltd.
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