BACKGROUND:We developed and evaluated a candidate reference measurement procedure (RMP) to standardize testosterone measurements, provide highly accurate and precise value assignments for the CDC Hormone Standardization Program, and ensure accurate and comparable results across testing systems and laboratories. METHODS:After 2 liquid/liquid extractions of serum with a combination of ethyl acetate and hexane, we quantified testosterone by isotope-dilution liquid chromatography-tandem mass spectrometry with electrospray ionization in the positive ion mode monitoring 289→97 m/z (testosterone) and 292→112 m/z ((3)C(13) testosterone). We used calibrator bracketing and gravimetric measurements to give higher specificity and accuracy to serum value assignments. The candidate RMP was evaluated for accuracy by use of NIST-certified reference material SRM971 and validated by split-sample comparison to established RMPs. We evaluated intraassay and interassay imprecision, measurement uncertainty, potential interferences, and matrix effects. RESULTS:A weighted Deming regression comparison of the candidate RMP to established RMPs showed agreement with no statistical difference (slope 0.99, 95% CI 0.98-1.00, intercept 0.54, 95% CI -1.24 to 2.32) and a bias of ≤0.3% for NIST SRM971. The candidate RMP gave maximum intraassay, interassay, and total percent CVs of 1.5%, 1.4%, and 1.7% across the concentrations of testosterone typically found in healthy men and women. We tested structural analogs of testosterone and 125 serum samples and found no interferences with the measurement. CONCLUSIONS:This RMP for testosterone can serve as a higher-order standard for measurement traceability and can be used to provide an accuracy base to which routine methods can be compared in the CDC Hormone Standardization Program.

译文

背景:我们开发并评估了候选参考测量程序(RMP),以标准化睾丸激素测量,为CDC激素标准化计划提供高度准确和精确的值分配,并确保在整个测试系统和实验室中获得准确和可比的结果。
方法:采用乙酸乙酯和己烷混合液两次液/液提取血清后,我们通过同位素稀释液相色谱-串联质谱在电离模式下以289→97 m / z(睾丸激素)进行电喷雾电离对睾丸激素进行定量。和292→112 m / z((3)C(13)睾丸激素)。我们使用了校准器包围和重量分析测量来为血清值分配提供更高的特异性和准确性。通过使用NIST认证的参考材料SRM971对候选RMP的准确性进行了评估,并通过与已建立的RMP的拆分样本比较进行了验证。我们评估了批内和批间不准确性,测量不确定度,潜在干扰和基质效应。
结果:候选RMP与已建立RMP的加权Deming回归比较显示无统计学差异(斜率0.99,95%CI 0.98-1.00,截距0.54,95%CI -1.24至2.32),偏差≤0.3% NIST SRM971。候选RMP在健康男性和女性通常存在的睾丸激素浓度范围内的最大批内,批间和CV总百分比分别为1.5%,1.4%和1.7%。我们测试了睾丸激素和125个血清样品的结构类似物,未发现对测量的干扰。
结论:该睾丸激素的RMP可以作为测量可追溯性的高级标准,并且可以用来为CDC激素标准化计划中的常规方法提供比较的准确性基础。

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