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Two-dimensional high performance liquid chromatography purification of underivatized urinary prednisone and prednisolone for compound-specific stable carbon isotope analysis
Analyst ( IF 3.6 ) Pub Date : 2024-07-26 , DOI: 10.1039/d4an00690a Zhongquan Li 1 , Bing Liu 1
Analyst ( IF 3.6 ) Pub Date : 2024-07-26 , DOI: 10.1039/d4an00690a Zhongquan Li 1 , Bing Liu 1
Affiliation
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The gas chromatography-combustion isotope ratio mass spectrometry (GC/C/IRMS) confirmation procedure for prednisone (PS) and prednisolone (PSL) is still a great challenge for the doping control laboratory due to the many structurally similar steroids present in urinary matrices. This study aims to establish an innovative online two-dimensional high performance liquid chromatography (2D-HPLC) purification method for measuring the carbon isotope ratios (CIRs) and achieving the identification of the synthetic forms of these two endogenous anabolic androgenic steroids (EAASs). Initially, the one-dimensional chromatographic column was used to separate and purify endogenous reference compounds (ERCs), and the co-elution fluids containing PS and PSL were switched to a two-dimensional chromatographic column for further purification through an online transfer system. Then the purified compounds were analyzed using GC/C/IRMS after sample pretreatments. The results showed that the minimum detection concentration of PS and PSL reached 30 ng mL−1, and no isotope fractionation occurred during the entire collection and preparation process. This method has been validated with the WADA technical document and showed good sensitivity and selectivity, demonstrating its practical applicability for urine samples in doping control laboratories.
中文翻译：
二维高效液相色谱纯化未衍生尿泼尼松和泼尼松龙，用于化合物特异性稳定碳同位素分析
由于尿液基质中存在许多结构相似的类固醇，泼尼松 (PS) 和泼尼松龙 (PSL) 的气相色谱-燃烧同位素比质谱 (GC/C/IRMS) 确认程序对于兴奋剂控制实验室来说仍然是一个巨大的挑战。本研究旨在建立一种创新的在线二维高效液相色谱（2D-HPLC）纯化方法，用于测量碳同位素比率（CIR）并实现这两种内源性合成代谢雄激素（EAAS）的合成形式的鉴定。最初使用一维色谱柱分离纯化内源性参考化合物（ERC），并将含有PS和PSL的共洗脱液通过在线传输系统切换至二维色谱柱进一步纯化。然后在样品预处理后使用 GC/C/IRMS 分析纯化的化合物。结果表明，PS和PSL的最低检测浓度达到30 ng mL -1 ，并且整个收集和制备过程中没有发生同位素分馏。该方法已通过WADA技术文件验证，表现出良好的灵敏度和选择性，证明了其在兴奋剂控制实验室尿液样本检测中的实际适用性。
更新日期：2024-07-26
中文翻译：
二维高效液相色谱纯化未衍生尿泼尼松和泼尼松龙，用于化合物特异性稳定碳同位素分析
由于尿液基质中存在许多结构相似的类固醇，泼尼松 (PS) 和泼尼松龙 (PSL) 的气相色谱-燃烧同位素比质谱 (GC/C/IRMS) 确认程序对于兴奋剂控制实验室来说仍然是一个巨大的挑战。本研究旨在建立一种创新的在线二维高效液相色谱（2D-HPLC）纯化方法，用于测量碳同位素比率（CIR）并实现这两种内源性合成代谢雄激素（EAAS）的合成形式的鉴定。最初使用一维色谱柱分离纯化内源性参考化合物（ERC），并将含有PS和PSL的共洗脱液通过在线传输系统切换至二维色谱柱进一步纯化。然后在样品预处理后使用 GC/C/IRMS 分析纯化的化合物。结果表明，PS和PSL的最低检测浓度达到30 ng mL -1 ，并且整个收集和制备过程中没有发生同位素分馏。该方法已通过WADA技术文件验证，表现出良好的灵敏度和选择性，证明了其在兴奋剂控制实验室尿液样本检测中的实际适用性。
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