Lee Ji Hyun, Park Han Na, Park Ok Rim, Kim Nam Sook, Park Sung-Kwan, Kang Hoil
Division of Advanced Analysis, Toxicological Evaluation and Research Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju-si, Chungcheongbuk-do, 28159, Republic of Korea.
Division of Advanced Analysis, Toxicological Evaluation and Research Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju-si, Chungcheongbuk-do, 28159, Republic of Korea.
Forensic Sci Int. 2019 May;298:10-19. doi: 10.1016/j.forsciint.2019.02.014. Epub 2019 Feb 22.
The worldwide spread of illegal sexual enhancement products is posing a threat to public health. The aim of this study was to investigate illegal products claiming to be effective in improving sexual performance through the online or offline markets between 2014 and 2017; these products include foods, dietary supplements, counterfeit drugs, and herbal medicines. These samples were analysed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the presence of 80 PDE-5 inhibitors (PDE-5i) and analogues. The developed method was validated as follows: LODs and LOQs spiked in solid- and liquid-type negative samples (0.03-3.33 ng/mL and 0.08-10.00 ng/mL), linearities (R > 0.997), recoveries spiked negative samples (82.2-109.3 %), accuracies (81.6-118.9 %), precisions (≥ 6.5%, RSD) of intra-day and inter-day, and stability (≥10.0%, RSD). Out of 362 measured samples, 145 were adulterated samples mostly detected in food (51%). Sildenafil group (50%) was frequently observed, followed by tadalafil group (41%). Although sildenafil and tadalafil were mainly detected in adulterated samples, their analogues were also found. In particular, new analogues have appeared steadily on illicit erectile dysfunction (ED) products even after they were first discovered. The concentration of detected samples ranged from 0.1 to 826.0 mg/g, and sildenafil of them contained a considerable amount in illicit ED products in 2014, posing a potential toxicology risk of public health. The testing method is fast and reliable making it suitable for both routine screening and up-to-date quantitative analysis of PDE-5i and their analogues in suspicious foods, dietary supplements, and counterfeit drugs.
非法性增强产品在全球范围内的传播正威胁着公众健康。本研究的目的是调查2014年至2017年期间通过线上或线下市场销售的声称对改善性功能有效的非法产品；这些产品包括食品、膳食补充剂、假药和草药。通过液相色谱-串联质谱法（LC-MS/MS）对这些样品进行分析，以检测80种磷酸二酯酶5抑制剂（PDE-5i）及其类似物的存在。所开发的方法按以下方式进行验证：在固体和液体类型的阴性样品中加标的检测限和定量限（0.03 - 3.33 ng/mL和0.08 - 10.00 ng/mL）、线性（R > 0.997）、加标阴性样品的回收率（82.2 - 109.3 %）、准确度（81.6 - 118.9 %）、日内和日间精密度（≥ 6.5%，RSD）以及稳定性（≥10.0%，RSD）。在362个被测样品中，有145个为掺假样品，大多在食品中检测到（51%）。西地那非组（50%）最为常见，其次是他达拉非组（41%）。虽然西地那非和他达拉非主要在掺假样品中检测到，但也发现了它们的类似物。特别是，新的类似物即使在首次被发现后，也不断出现在非法勃起功能障碍（ED）产品中。检测样品的浓度范围为0.1至826.0 mg/g，其中西地那非在2014年的非法ED产品中含量相当可观，对公众健康构成潜在的毒理学风险。该检测方法快速可靠，适用于对可疑食品、膳食补充剂和假药中的PDE-5i及其类似物进行常规筛查和最新的定量分析。
