The presence of plant toxins and/or cyanotoxins in food supplements implies consumer health risks. Therefore, a targeted ultra-high performance liquid chromatographic-tandem mass spectrometric method to detect/quantify 25 toxins simultaneously in food supplement formulations was developed and validated. Full validation for tablets/powders and secondary validation for a liquid and soft gel capsule indicated that most compounds were efficiently extracted (≥ 75%), while others were only partly extracted (18 – 61%). Trueness was fulfilled (70 – 120%), with some exceptions (mostly at the lowest validation level). Intralaboratory repeatability, intra- and interlaboratory reproducibility values of ≤ 20%, ≤ 25%, and ≤ 25% were obtained for most, respectively. Matrix effects were found to be significant for most compounds. Good sensitivity (µg/kg level) was observed for galegin(e), lycopsamine, lycorine, rubiadin, skimmiamine, and vascin(e), in contrast to helveticoside, lucidin, lucidin-3-primveroside, plumbagin(e), and thujone, which were detected at the mg/kg level. The other compounds were characterized by a sensitivity between 10 to 1000 µg/kg. The validated methodology was applied for 52 food supplements (tablets, capsules, liquids/syrup, etc.) purchased from the Belgian market. In more than 25% of the samples, one or more toxins were detected (concentrations determined using standard addition). Lycopsamine, microcystin LR, solamargine, thujone, and vasicin(e) were the most frequently detected toxins. A clear link between the toxins detected and the plant species on the food supplement ingredient list could not always be established. This generic “dilute-and-shoot” procedure can be used for further research on toxins in food supplements and by extension other plant/algae-based food/feed commodities (herbs, edible flowers, etc.).

中文翻译：

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食品补充剂中植物毒素和蓝藻毒素的多级 UHPLC-MS/MS 方法及其在比利时市场样品中的应用

食品补充剂中存在植物毒素和/或蓝藻毒素意味着消费者的健康风险。因此，开发并验证了一种有针对性的超高效液相色谱-串联质谱方法，可同时检测/量化食品补充剂配方中的 25 种毒素。片剂/粉末的全面验证和液体和软胶囊的二次验证表明大多数化合物被有效提取（≥ 75%），而其他化合物仅被部分提取（18 – 61%）。真实性得到满足（70 – 120%），但有一些例外（主要是在最低验证级别）。大多数人分别获得了≤20%、≤25%和≤25%的实验室内重复性、实验室内和实验室间重复性值。发现大多数化合物的基质效应是显着的。与 helveticoside、lucidin、lucidin-3-primveroside、plumbagin(e) 和 thujone 相比，对半乳糖苷 (e)、lycopsamine、lycorine、rubiadin、skimmiamine 和 vascin(e) 观察到良好的灵敏度（µg/kg 水平） ，以 mg/kg 水平检测。其他化合物的特点是灵敏度在 10 到 1000 µg/kg 之间。经验证的方法应用于从比利时市场购买的 52 种食品补充剂（片剂、胶囊、液体/糖浆等）。在超过 25% 的样品中，检测到一种或多种毒素（使用标准添加确定浓度）。番茄红素、微囊藻毒素 LR、solamargin、thujone 和 vasicin(e) 是最常检测到的毒素。检测到的毒素与食品补充剂成分表上的植物物种之间的明确联系并不总是能建立起来。