In this work, liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed and validated for screening and confirmation of 64 illicit compounds in dietary supplements. The target compounds were illegally used pharmaceutical drugs, prohibited compounds, and not authorized ingredients for different therapeutics (sexual enhancement, weight loss, muscular strengthening, and relaxing products). The validation procedure was performed to evaluate selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision according to the Association of Official Analytical Chemists guidelines. The linearity was >0.98 in the range of 0.5–200 µg L−1. The LOQs were in the range 1–10 µg kg−1 for all target compounds. The accuracy (expressed as recovery) was 78.5–114%. The precision (expressed as the relative standard deviation) was below 9.15%. The developed method was applied for the determination of illicit compounds in dietary supplements collected from websites. As a result, the total detection rate was 13.5% (27 samples detected in 200 samples). The concentrations of detected samples ranged from 0.51 to 226 mg g−1. The proposed methodology is suitable for monitoring the adulteration of illicit compounds in dietary supplements.

中文翻译：

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使用液相色谱-串联质谱法对膳食补充剂中的 64 种违禁化合物进行多类别测定

在这项工作中，开发并验证了液相色谱-串联质谱 (LC-MS/MS) 方法，用于筛查和确认膳食补充剂中的 64 种非法化合物。目标化合物是非法使用的药物、禁用化合物和不同疗法（性增强、减肥、肌肉增强和放松产品）的未授权成分。根据官方分析化学家协会的指南，执行验证程序以评估选择性、线性、检测限 (LOD)、定量限 (LOQ)、准确度和精密度。在 0.5–200 µg L-1 范围内，线性度 >0.98。所有目标化合物的 LOQ 范围为 1–10 µg kg-1。准确度（以回收率表示）为 78.5-114%。精密度（表示为相对标准偏差）低于 9.15%。所开发的方法用于测定从网站收集的膳食补充剂中的非法化合物。结果总检出率为13.5%（200个样本中检出27个样本）。检测到的样品浓度范围为 0.51 至 226 mg g-1。建议的方法适用于监测膳食补充剂中非法化合物的掺假。