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Investigations into the analysis of intact drug conjugates in animal sport doping control - Development and assessment of a rapid and economical approach for screening greyhound urine.
Drug Testing and Analysis ( IF 2.6 ) Pub Date : 2020-02-21 , DOI: 10.1002/dta.2779
Bob Gray 1, 2 , Lisa Tuckley 1 , Charlotte Cutler 1 , Simon Biddle 1 , Simon Hudson 1 , Simon Gower 3 , Lynn Vanhaecke 2, 4
Affiliation  

Animal sport doping control laboratories are constantly reviewing ways in which they can improve their service offering whilst ensuring that they remain economically viable. This paper describes the development and assessment of a rapid and economical method for the detection of intact glucuronide conjugates of three anabolic steroids and their metabolites along with three corticosteroids in canine urine. The analysis of intact drug conjugates for animal sport doping control is generally not performed routinely as it presents a number of analytical challenges, not least of which is the lack of availability of appropriate reference standards. Here, we report the development of a UHPLC–MS/MS method using APCI in the negative ion mode for the detection of intact phase II conjugates, including the importance of in vitro incubations in order to provide appropriate reference materials. Cross‐validation of the developed method demonstrated that the detection capability of the intact phase II conjugates of stanozolol, boldenone, nandrolone, and their metabolites along with the corticosteroids dexamethasone and methylprednisolone was equivalent to that achieved in routine race‐day screens. The new process has been in operation for approximately 2 years and has been used to analyze in excess of 13500 canine urine samples, resulting in a number of positive screening findings. To the best of our knowledge, this is the first reported use of a routine screen for intact drug conjugates within animal sport doping control.

中文翻译:

在动物运动兴奋剂控制中分析完整药物共轭物的研究-快速和经济的灰狗尿液筛查方法的开发和评估。

动物运动兴奋剂控制实验室正在不断审查可以改善服务质量同时确保其经济可行性的方法。本文描述了一种快速经济的方法,用于检测犬尿中三种合成代谢类固醇及其代谢产物以及三种皮质类固醇的完整葡糖苷酸结合物的开发和评估。用于动物运动兴奋剂控制的完整药物偶联物的分析通常不常规进行,因为它带来了许多分析难题,尤其是缺乏适当参考标准的问题。在这里,我们报告了使用APCI以负离子模式检测完整的II期结合物的UHPLC-MS / MS方法的发展,包括体外培养的重要性,以提供适当的参考材料。所开发方法的交叉验证表明,完整的stanozolol,Boldenone,nandrolone及其代谢物的II期结合物以及皮质类固醇地塞米松和甲基强的松龙的检测能力与常规比赛日筛查相当。新工艺已经运行了大约2年,已经用于分析超过13500种犬尿液样品,从而产生了许多积极的筛查结果。据我们所知,这是首次报道在动物运动兴奋剂控制中使用常规筛查完整药物结合物的方法。所开发方法的交叉验证表明,完整的stanozolol,Boldenone,nandrolone及其代谢物的II期结合物以及皮质类固醇地塞米松和甲基强的松龙的检测能力与常规比赛日筛查相当。新工艺已经运行了大约2年,已经用于分析超过13500种犬尿液样品,从而产生了许多积极的筛查结果。据我们所知,这是首次报道在动物运动兴奋剂控制中使用常规筛查完整药物结合物的方法。所开发方法的交叉验证表明,完整的stanozolol,Boldenone,nandrolone及其代谢物的II期结合物以及皮质类固醇地塞米松和甲基强的松龙的检测能力与常规比赛日筛查相当。新工艺已经运行了大约2年,已经用于分析超过13500种犬尿液样品,从而产生了许多积极的筛查结果。据我们所知,这是首次报道在动物运动兴奋剂控制中使用常规筛查完整药物结合物的方法。新工艺已经运行了大约2年,已经用于分析超过13500种犬尿液样品,从而产生了许多积极的筛查结果。据我们所知,这是首次报道在动物运动兴奋剂控制中使用常规筛查完整药物结合物的方法。新工艺已经运行了大约2年,已经用于分析超过13500种犬尿液样品,从而产生了许多积极的筛查结果。据我们所知,这是首次报道在动物运动兴奋剂控制中使用常规筛查完整药物结合物的方法。
更新日期:2020-02-21
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