Ultraviolet spectra determination and computational analysis of 44 E/Z steroid isomers in dried blood spot

Author:

Yan Xiya12ORCID,Yan Siyu12,Chang Wei2ORCID,Wen Chao2,Zhang Lisi2,Wang Zhanliang2,Yang Sheng2

Affiliation:

1. School of Sport Science Beijing Sport University Beijing China

2. Beijing Anti‐Doping Laboratory Beijing Sport University Beijing China

Abstract

AbstractThe dried blood spot (DBS) is a novel alternative matrix used in 2022 Beijing Winter Olympics and Paralympics. It is capable of distinguishing anabolic androgenic steroid (AAS) esters without the gas chromatography–combustion–isotope ratio mass spectrometry (GC‐C‐IRMS) confirmation. In this study, a method for detection of 22 anabolic steroid esters in DBS based on ultra‐high liquid chromatography–mass spectrometry (UPLC‐MS) with parallel reaction monitoring (PRM) was developed and validated. Methoxylamine was used as the derivatization reagent to improve the sensibility. Specificity, limit of detection (LOD), linearity, stability, robustness, and carryover were evaluated. Steroid esters are nine testosterone esters, six nandrolone esters, five boldenone esters, methenolone enanthate, and trenbolone acetate. UV spectra were determined by HPLC. And density functional theory (DFT) calculation methods could provide theoretical UV spectra data. Three basis set of B3LYP/6‐31G(d), B3LYP/6‐31+G(d, p), and WB97XD/6‐31+G(d, p) were used for the geometry optimizations and TD‐DFT calculation. The average deviation (%RD) of B3LYP/6‐31+G(d) for all 44 ester oximes are less than 3.0%. This study for the first time provides a method to tentatively identify the 44 E/Z configurations of steroid oxime products.

Publisher

Wiley

Subject

Spectroscopy,Pharmaceutical Science,Environmental Chemistry,Analytical Chemistry

Reference36 articles.

1. World Anti‐Doping Agency.Anti‐doping testing figures Montreal.2021. Accessed August 5 2023.https://www.wada-ama.org/sites/default/files/2023-01/2021_anti-doping_testing_figures_en.pdf

2. The Effects of Supraphysiologic Doses of Testosterone on Muscle Size and Strength in Normal Men

Cited by 1 articles. 订阅此论文施引文献 订阅此论文施引文献,注册后可以免费订阅5篇论文的施引文献,订阅后可以查看论文全部施引文献

同舟云学术

1.学者识别学者识别

2.学术分析学术分析

3.人才评估人才评估

"同舟云学术"是以全球学者为主线,采集、加工和组织学术论文而形成的新型学术文献查询和分析系统,可以对全球学者进行文献检索和人才价值评估。用户可以通过关注某些学科领域的顶尖人物而持续追踪该领域的学科进展和研究前沿。经过近期的数据扩容,当前同舟云学术共收录了国内外主流学术期刊6万余种,收集的期刊论文及会议论文总量共计约1.5亿篇,并以每天添加12000余篇中外论文的速度递增。我们也可以为用户提供个性化、定制化的学者数据。欢迎来电咨询!咨询电话:010-8811{复制后删除}0370

www.globalauthorid.com

TOP

Copyright © 2019-2024 北京同舟云网络信息技术有限公司
京公网安备11010802033243号  京ICP备18003416号-3