Reliable identification and quantification of anabolic androgenic steroids in dietary supplements by using gas chromatography coupled to triple quadrupole mass spectrometry.,Drug Testing and Analysis

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Reliable identification and quantification of anabolic androgenic steroids in dietary supplements by using gas chromatography coupled to triple quadrupole mass spectrometry.
Drug Testing and Analysis ( IF 2.6 ) Pub Date : 2020-09-22 , DOI: 10.1002/dta.2929
Giuseppe Micalizzi ₁ , Katalin Huszti ₂ , Zoltán Pálinkás ₂ , Filippo Mandolfino _{1,

3} , Éva Martos ₂ , Paola Dugo _{1,

4} , Luigi Mondello _{1,

4,

5,

6} , Margita Utczás _{2,

4}

Affiliation

The aim of the present research was the identification and quantification of specific anabolic androgenic steroids (AASs) and other sterane structured compounds in dietary supplements (DSs). The adulteration of DSs by these compounds is of a particular concern in athletes, because it might lead to a positive doping result. The research was focused on the optimization of a highly sensitive and selective GC‐based analytical strategy using triple quadrupole MS as detector. Chromatographic method and multiple reaction monitoring (MRM) transitions of 28 target compounds were optimized. Sample clean‐up was carried out by using a solid phase extraction (SPE) procedure, while the derivatization of AASs was performed by using N‐methyl‐N‐(trimethylsilyl)‐trifluoroacetamide (MSTFA). The method was validated, and the following parameters were investigated: linearity range, limit of detection, accuracy, and precision expressed in terms of intra‐day precision. The calibration curves were evaluated by using regression model and resulting in a good determination coefficients (R² ≥ 0.9912). The residuals were scattered randomly around zero. The limits of detection (LODs) were lower than 7.0 ng g⁻¹ or ng ml⁻¹. The accuracy assessment was evaluated in different forms of DSs characterized by high sample‐to‐sample variability (liquid, powder, tablet, capsule, protein, and herbal‐based). Intra‐day assay precision was in all cases lower than 20%. The developed analytical method was successfully applied to the analysis of 67 commercially available dietary supplements. In five cases, one or more steroid‐type compounds were found in the concentration of 5 ng g⁻¹–100 μg g⁻¹, which might result adverse analytical findings in athletes.

中文翻译：

使用气相色谱与三重四极杆质谱联用对膳食补充剂中的合成代谢雄激素类固醇进行可靠的鉴定和定量。

本研究的目的是鉴定和量化膳食补充剂 (DS) 中特定的合成代谢雄激素 (AAS) 和其他甾烷结构化合物。这些化合物掺入 DSs 是运动员特别关注的问题，因为这可能会导致兴奋剂结果呈阳性。该研究的重点是使用三重四极杆 MS 作为检测器优化基于 GC 的高灵敏度和选择性分析策略。优化了 28 种目标化合物的色谱方法和多反应监测 (MRM) 离子对。使用固相萃取 (SPE) 程序进行样品净化，而使用N-甲基-N进行 AAS 的衍生化-（三甲基甲硅烷基）-三氟乙酰胺（MSTFA）。对该方法进行了验证，并研究了以下参数：线性范围、检测限、准确度和以日内精密度表示的精密度。使用回归模型对校准曲线进行评估，得出了良好的决定系数（R ² ≥ 0.9912）。残差随机散布在零附近。检测限 (LOD) 低于 7.0 ng g ^-1或 ng ml ^-1. 准确性评估在不同形式的 DSs 中进行评估，这些 DSs 具有较高的样本间变异性（液体、粉末、片剂、胶囊、蛋白质和基于草药）。在所有情况下，日内检测精度均低于 20%。开发的分析方法已成功应用于 67 种市售膳食补充剂的分析。在五个案例中，发现一种或多种类固醇类化合物的浓度为 5 ng g ^-1 –100 μg g ^-1，这可能会导致运动员的不良分析结果。

更新日期：2020-09-22

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