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高容量类固醇同位素标准品被开发用作气相色谱-燃烧-同位素比率质谱分析法的工作标准品。

High-volume steroid isotopic standards developed as working standards for gas chromatography-combustion-isotope ratio mass spectrometry.

作者信息

Tobias Herbert J, Brenna J Thomas

机构信息

Division of Nutritional Sciences, Cornell University, Ithaca, New York.

Dell Pediatric Research Institute, Dell Medical School, University of Texas at Austin, Austin, Texas, USA.

出版信息

Drug Test Anal. 2018 Apr;10(4):781-785. doi: 10.1002/dta.2309. Epub 2017 Nov 13.

Abstract

High-precision carbon isotope ratio analysis of urinary steroids by gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) is the official test to detect illicit doping of synthetic versions of endogenous steroids, such as testosterone. Our group created the first steroid isotopic standards (SIS) specifically for World Anti-Doping Agency (WADA) accredited laboratories. The standards contain mixtures of steroids as acetates or free steroids at ~400 μg each per ampoule and have been widely distributed to anti-doping laboratories to facilitate comparability of inter-laboratory results. Here we report on the creation and characterization of 3 new high-volume single component SIS suitable for use as working standards. They contain ~50 times more steroid mass per ampoule than previous SIS. The new SIS, coded CU/PCC 40-1, CU/PCC 41-1, & CU/PCC 42-1, contain ~20 mg of androsterone, androsterone-AC, and 5α-cholestane, with determined isotopic values of -27.09 ± 0.07 mUr, -32.82 ± 0.01 mUr, -25.03 ± 0.01 mUr, respectively. We used our previously developed protocol to calibrate the isotopically uniform steroids against the isotopic standard gases methane and ethane in NIST RM 8559 that are traceable to the international standard Vienna PeeDee Belemnite (VPDB). Two sets of data, acquired 7 months apart, of absolute δ C and ∆Δδ C values from 8 randomly selected ampoules of all 3 SIS indicate uniformity of steroid isotopic composition within measurement reproducibility, SD(δ C) < 0.2 mUr Our results show that protocols for SIS extend to creation of high volume working standards that can also be used as internal standards under appropriate GC conditions.

摘要

采用气相色谱-燃烧-同位素比率质谱法(GC-C-IRMS)对尿类固醇进行高精度碳同位素比率分析,是检测内源性类固醇(如睾酮)合成版本非法使用兴奋剂的官方检测方法。我们团队创建了首个专门用于世界反兴奋剂机构(WADA)认可实验室的类固醇同位素标准品(SIS)。这些标准品包含醋酸盐形式或游离类固醇形式的类固醇混合物,每安瓿约含400μg,已广泛分发给反兴奋剂实验室,以促进实验室间结果的可比性。在此,我们报告3种新型大容量单一组分SIS的创建及特性,这些SIS适合用作工作标准品。它们每安瓿所含类固醇质量比先前的SIS多约50倍。新的SIS编码为CU/PCC 40-1、CU/PCC 41-1和CU/PCC 42-1,分别含有约20mg的雄甾酮、雄甾酮-AC和5α-胆甾烷,其测定的同位素值分别为-27.09±0.07 mUr、-32.82±0.01 mUr、-25.03±0.01 mUr。我们使用先前开发的方案,以可溯源至国际标准维也纳皮迪迪贝莱姆石(VPDB)的NIST RM 8559中的同位素标准气体甲烷和乙烷为参照,对同位素均匀的类固醇进行校准。从所有3种SIS的8个随机选择的安瓿中获取的两组间隔7个月的绝对δC和∆∆δC值数据表明,类固醇同位素组成在测量再现性范围内具有均匀性,SD(δC) < 0.2 mUr。我们的结果表明,SIS方案可扩展至创建大容量工作标准品,在适当的气相色谱条件下,这些标准品也可用作内标。

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