Validity of Free Testosterone and Free Estradiol Determinations in Serum Samples from Postmenopausal Women by Theoretical Calculations Sabina Rinaldi, Annabelle Geay, Henri De ´chaud, Carine Biessy, Anne Zeleniuch-Jacquotte, Arslan Akhmedkhanov, Roy E. Shore, Elio Riboli, Paolo Toniolo, and Rudolf Kaaks 1 IARC, Unit of Nutrition and Cancer, 69500 Lyon, France [S. R., C. B., E. R., R. K.]; Service de Radioanalyse et Radiopharmacie, Ho ˆpital Neuro- cardiologique, Hospices Civils de Lyon, Lyon, France [A. G., H. D.]; and Departments of Environmental Medicine [A. Z-J., A. A., R. E. S., P. T.] and Obstetrics and Gynecology [A. A., P. T.], New York University School of Medicine, New York, New York 10010 Abstract In this study, we validated measurements of free testosterone (fT) and free estradiol (fE 2 ) concentrations calculated from total serum concentrations of testosterone (T), estradiol (E 2 ), and sex hormone-binding globulin (SHBG), measured by direct, commercial radioimmunoassays, by comparison with reference measurements obtained by dialysis plus an in-house radioimmunoassay after extraction and chromatographic purification. The study was conducted in serum samples from 19 postmenopausal women who were part of an ongoing prospective cohort study. We also performed sensitivity analyses to examine the robustness of the theoretical calculations. Sensitivity analyses showed that in this population, competitive binding of dihydrotestosterone and total T could be ignored in the calculation of fE 2 , and competitive binding by dihydrotestosterone does not need to be taken into account for calculation of fT. Furthermore, variations in albumin and SHBG concentrations had negligible effects on fT and fE 2 calculations. Values of fT and fE 2, calculated from total T and E 2 concentrations obtained by the same in-house radioimmunoassay used for the dialysis method, correlated highly with the measurements by dialysis (Pearson’s coefficients of correlation above 0.97). When calculating fT and fE 2 using total T and total E 2 concentrations obtained by different direct radioimmunoassays, almost all kits gave good correlations with the reference method for fT (Pearson’s r > 0.83), but only a few gave good correlations for fE 2 (Diagnostic System Laboratories and DiaSorin; r > 0.80). The direct radioimmunoassays giving the best correlation for fT and fE 2 with the dialysis method were those that best measured total concentrations of T and E 2 . Furthermore, mean values of fT and fE 2 corresponded well to mean values by the reference method if SHBG measurements were also well calibrated. We conclude that in postmenopausal women, theoretical calculations are valid for the determination of fT and fE 2 concentrations and can give reliable estimation of cancer risk in epidemiological studies when the total concentrations of T, E 2 , and SHBG are measured accurately. Introduction Epidemiological studies have shown relationships of breast and endometrial cancers with concentrations of T 2 and E 2 in blood among postmenopausal women (1–3). Both T and E 2 are trans- ported in blood bound to proteins (4, 5), of which the most important are albumin and SHBG. Together, these proteins bind 97% of T and E 2 circulating in blood (6). The percentage of T and E 2 that circulates either free (i.e., unbound to any protein) or bound to albumin is defined as the “bioavailable fraction” because only this fraction can potentially cross cellu- lar membranes and bind to the nuclear steroid receptors (7). The bioavailable fraction is virtually equal to the fraction not linked to SHBG (8) and represents 50% of total E 2 and 30% of total T in normal women and men (9). fT and fE 2 are most directly available to tissues under physiological conditions and generally correlate strongly with concentrations of T and E 2 unbound to SHBG (8). To clarify the roles of fT and fE 2 (and therefore of their bioavailable fractions) in the development of cancer in post- menopausal women, it is important to have precise and inex- pensive methods for their measurement that can be easily applied to large-scale epidemiological studies. Several methods have been set up for the measurement of fT and fE 2 rather than for the measurement of the bioavailable fractions because in normal subjects, the free and bioavailable fractions are very highly correlated (8), and the methods for the measurement of the T and E 2 bioavailable fractions require a large amount of biological sample (10 –12). The most common methods for measurement of fT and fE 2 are based on dialysis (13, 14), ultrafiltration (15–18), and gel filtration (19, 20). These meth- ods do not measure the absolute concentrations of fT and fE 2 directly but measure fT and fE 2 as percentages of the total circulating T and E 2 concentrations. Absolute levels of fT and fE 2 are then determined by multiplying the percentage of fT or fE 2 with measurements of total T and E 2 , respectively (13). Gel Received 2/4/02; revised 5/17/02; accepted 5/29/02. The costs of publication of this article were defrayed in part by the payment of page charges. This article must therefore be hereby marked advertisement in accordance with 18 U.S.C. Section 1734 solely to indicate this fact. 1 To whom requests for reprints should be addressed, at IARC, Unit of Nutrition and Cancer, 150 Cours Albert Thomas, 69372 Lyon, France. Fax: 33-04-72-73- 85-75. 2 The abbreviations used are: T, testosterone; fT, free testosterone; E 2 , estradiol; fE 2 , free estradiol; SHBG, sex hormone-binding globulin; DHT, dihydrotestos- terone; fDHT, free dihydrotestosterone; CI, confidence interval. 1065 Vol. 11, 1065–1071, October 2002 Cancer Epidemiology, Biomarkers & Prevention on January 8, 2022. © 2002 American Association for Cancer Research. cebp.aacrjournals.org Downloaded from