Page 63 - Clinical-Medical Solution for Clinical Chemistry

LAAN-A-LM-E113$

Application Liquid Chromatography Mass Spectrometry

News Screening Analysis of Highly Polar Doping Agents

in Urine Using 2DLC/MS/MS
No.C142$

The use of performance-enhancing drugs, or "doping," as well as the emergence of designer drugs and the
has been recognised for decades and since 1999 the manipulation of blood and blood components results in
World Anti-Doping Agency (WADA) has governed and sports drug testing methods which are capable of a
harmonized the worldwide sports drug testing efforts. range of tests. In this application news, we report the
However, these needs are changing and the continuing. simultaneous analysis of highly polar doping agents
discovery of new doping strategies with naturally including meldonium and adrenergic agents such as
occurring substances, such as androgenic steroids, pro- synephrine, norfenefrine, etilefrine, oxilofrine and
hormones and related metabolites, peptide hormones, octopamine using 2D LC/MS/MS

[Anti-ischemic drug] [Adrenergic agents]
Meldonium
Synephrine Etilefrine

Formula: C6H14N2O2
Exact Mass: 146.1055
Formula: C9H13NO2 Formula: C10H15NO2
Exact Mass: 167.0946 Exact Mass: 181.1103
Oxilofrine Norfenefrine Octopamine

Formula: C10H15NO2 Formula: C8H11NO2 Formula: C8H11NO2
Exact Mass: 181.1103 Exact Mass: 153.079 Exact Mass: 153.079

Fig. 1 Structures of 6 Compounds

Table 1 Analytical Conditions
[LC] NexeraX2 System [MS] LCMS-8060
Analytical Column : Nucleodur HILIC (100 mm L. × 2 mm I.D., 1.8 μm) Ionization : ESI (+/-)
Trapping Column : Nucleodur HILIC (20 mm L. × 2 mm I.D., 3 μm) Nebulizing Gas Flow : 3.0 L/min.
Mobile Phase : A: H 2 O + 5 % buffer, Drying Gas Flow : 15.0 L/min.
B: Acetonitrile + 5 % buffer, Heating Gas Flow : 15.0 L/min.
C: Acetonitrile + 5 % buffer HB Temp. : 500 ˚C
(buffer: 200 mM Ammonium Acetate + 0.15 % DL Temp. : 300 ˚C
glacial acetic acid) Interface Temp. : 400 ˚C
Column Oven Temp. : 40 ˚C
Injection Volume : 30 μL