Center for Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju-si, Chungcheongbuk-do, Republic of Korea.
Rapid Commun Mass Spectrom. 2022 Apr 30;36(8):e9275. doi: 10.1002/rcm.9275.
Dietary supplements advertised to strengthen muscles have earned fame among athletes. However, several products containing unauthorized compounds are often detected, which can cause a public health risk. Particularly, steroids and selective androgen receptor modulators (SARMs) can cause serious side effects as hormone modulators. In this study, we analyzed 15 steroids and 20 SARMs using liquid chromatography-quadrupole time-of-flight mass spectrometry (LC/QTOFMS) to provide fundamental information about fragmentation pathways and fragment ion structures.
The optimal conditions of LC/QTOFMS were explored to obtain fragmentation patterns for each compound. The optimal conditions were established by comparing the area and height of the precursor ion peak at 125 or 175 V as a fragmentor energy. Furthermore, the optimized spectra were acquired by applying collision energy ranging from 1 to 50 eV. The energy value was selected under the condition that the mass error of precursor ions was less than 10 ppm.
The 35 compounds were classified on the basis of their chemical core structures: arylpropionamide (3 compounds), quinolinone (2), pyrrolidinylbenzonitrile (1), indole (2), tropanol (2), phenylaxadaizole (1), hydantoin (2), phenylthiazole (1), nitrothiophene (1) and steroidal derivative (20). Fragmentation pathways and the chemical structure of each product ion were predicted and identified. Furthermore, the obtained structural information was applied to screen seized samples. As a result, 10 seized samples were confirmed to contain one or more SARMs by comparing each precursor ion and fragmentation pattern.
The application to real samples for accurate screening indicated that the same fragmentation patterns and product ions as one or more SARM standards were detected and identified in the seized samples advertised as muscle building. Therefore, this study can contribute to ensuring the safety of public health through providing fundamental information about the risk of illegal adulteration.
宣传可增强肌肉的膳食补充剂在运动员中声名鹊起。然而，经常检测到含有未经授权化合物的几种产品，这可能会对公众健康造成风险。特别是类固醇和选择性雄激素受体调节剂 (SARMs) 作为激素调节剂会引起严重的副作用。在这项研究中，我们使用液相色谱-四极杆飞行时间质谱 (LC/QTOFMS) 分析了 15 种类固醇和 20 种 SARMs，为化合物的断裂途径和碎片离子结构提供了基本信息。
探索了 LC/QTOFMS 的最佳条件，以获得每种化合物的断裂模式。通过比较作为碎片器能量的 125 或 175V 处的前体离子峰的面积和高度来确定最佳条件。此外，通过应用从 1 到 50eV 的碰撞能量来获得优化的光谱。选择前体离子质量误差小于 10ppm 的条件下的能量值。
根据其化学核心结构对 35 种化合物进行分类：芳基丙酰胺（3 种）、喹啉酮（2 种）、吡咯烷基苯甲腈（1 种）、吲哚（2 种）、托烷（2 种）、苯并哒嗪（1 种）、海因（2 种）、噻唑（1 种）、硝基噻吩（1 种）和甾体衍生物（20 种）。预测并鉴定了每种产物离子的断裂途径和化学结构。此外，获得的结构信息被应用于筛选扣押样品。结果，通过比较每种前体离子和断裂模式，在宣传为增肌的扣押样品中确认了 10 个扣押样品含有一种或多种 SARMs。
对实际样品进行准确筛选的应用表明，在宣传为增肌的扣押样品中检测到并鉴定出与一种或多种 SARM 标准相同的断裂模式和产物离子。因此，本研究通过提供有关非法掺假风险的基本信息，有助于确保公众健康的安全。
