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Articles |
1
UCLA Olympic Analytical Laboratory, Department of Molecular and Medical Pharmacology and
2
Department of Medicine, University of California at Los Angeles, Los Angeles, CA 90025.
3
The word "elevated" is used to refer to a result that is above the administrative cutoff.
a Address correspondence to this author at: UCLA Olympic Analytical Laboratory, Department of Molecular and Medical Pharmacology, University of California at Los Angeles, 2122 Granville Ave., Los Angeles, CA 90025-6106. Fax 310-206-9077; e-mail
rodrigoa{at}ucla.edu.
Background: Carbon isotope ratio methods are used in doping control to determine whether urinary steroids are endogenous or pharmaceutical.
Methods: Gas chromatography-combustion-isotope ratio mass
spectrometry (GC-C-IRMS) was used to determine the
13C
values for 5{beta}-androstane-3
,17{beta}-diyl diacetate (5{beta}A),
5
-androstane-3
,17{beta}-diyl diacetate (5
A), and
5{beta}-pregnane-3
,20
-diyl diacetate (5{beta}P) in a control group of
73 healthy males and 6 athletes with testosterone/epitestosterone
ratios (T/E) >6.
Results: The within-assay precision SDs for 5{beta}A, 5
A, and
5{beta}P were ± 0.27
, ± 0.38
, and ± 0.28
,
respectively. The between-assay precision SDs ranged from ±
0.40
to ± 0.52
. The system suitability and batch acceptance
scheme is based on SDs. For the control group, the mean
13C (SD) values were -25.69
(± 0.92
),
-26.35
(± 0.68
), and -24.26
(± 0.70
), for 5{beta}A, 5
A,
and 5{beta}P, respectively. 5{beta}P was greater than 5{beta}A and 5
A
(P <0.01), and 5{beta}A was greater than 5
A
(P <0.01). The means - 3 SD were -28.46
,
-28.39
, and -26.37
for 5{beta}A, 5
A, and 5{beta}P, respectively.
The maximum difference between 5{beta}P and 5{beta}A was 3.2
, and
the maximum 5{beta}A/5{beta}P was 1.13. Three athletes with chronically
elevated T/Es had
13C values consistent with
testosterone administration and three did not.
Conclusions: This GC-C-IRMS assay of urine diols has low within-
and between-assay SDs; therefore, analysis of one urine sample suffices
for doping control. The means, SDs, ±3 SDs, and ranges of
13C values in a control group are established. In
comparison, testosterone users have low 5{beta}A and 5
A, large
differences between 5{beta}A or 5
A and 5{beta}P, and high 5{beta}A/5{beta}P and
5
A/5{beta}P ratios.
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