Doping in sport-2. Quantification of the impurity 19-norandrostenedione in pharmaceutical preparations of norethisterone

TY - JOUR

T1 - Doping in sport-2. Quantification of the impurity 19-norandrostenedione in pharmaceutical preparations of norethisterone

AU - Walker, Christopher J.

AU - Cowan, David A.

AU - James, Vivian H. T.

AU - Lau, Joanne C. Y.

AU - Kicman, Andrew T.

PY - 2009/3

Y1 - 2009/3

N2 - The finding of measurable amounts of 19-norandrostenedione in norethisterone tablets prompted us to develop an assay to quantify this steroid. 19-Norandrostenedione is an anabolic steroid whose use in sport is prohibited by the World Anti-Doping Agency (WADA). The assay was developed using isotope dilution and liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the quantification of 19-norandrostenedione in norethisterone formulations, with [3,4(-13)C(2)]-19-norandrostenedione as the internal standard. The results showed amounts up to 1.01 +/- 0.01 mu g (mean +/- S.E.M.) per tablet in those containing S mg of norethisterone or norethisterone acetate (0.02%, w/w) and up to 0.5 +/- 0.01 mu g (mean S.E.M.) per tablet (0.05%, w/w) in oral contraceptive tablets containing 0.35-1.5 mg of norethisterone or norethisterone acetate. No tablet tested exceeded the British Pharmacopoeia limit of 0.1% for this impurity. (C) 2008 Elsevier Inc. All rights reserved.

AB - The finding of measurable amounts of 19-norandrostenedione in norethisterone tablets prompted us to develop an assay to quantify this steroid. 19-Norandrostenedione is an anabolic steroid whose use in sport is prohibited by the World Anti-Doping Agency (WADA). The assay was developed using isotope dilution and liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the quantification of 19-norandrostenedione in norethisterone formulations, with [3,4(-13)C(2)]-19-norandrostenedione as the internal standard. The results showed amounts up to 1.01 +/- 0.01 mu g (mean +/- S.E.M.) per tablet in those containing S mg of norethisterone or norethisterone acetate (0.02%, w/w) and up to 0.5 +/- 0.01 mu g (mean S.E.M.) per tablet (0.05%, w/w) in oral contraceptive tablets containing 0.35-1.5 mg of norethisterone or norethisterone acetate. No tablet tested exceeded the British Pharmacopoeia limit of 0.1% for this impurity. (C) 2008 Elsevier Inc. All rights reserved.

U2 - 10.1016/j.steroids.2008.10.006

DO - 10.1016/j.steroids.2008.10.006

M3 - Article

VL - 74

SP - 335

EP - 340

JO - Steroids

JF - Steroids

IS - 3

ER -