Institute of Plant Protection - National Research Institute, Chełmońskiego 22, 15-195 Bialystok, Poland.
Institute of Plant Protection - National Research Institute, Chełmońskiego 22, 15-195 Bialystok, Poland.
J Pharm Biomed Anal. 2020 Aug 5;187:113351. doi: 10.1016/j.jpba.2020.113351. Epub 2020 May 5.
Pyrrolizidine alkaloids (PAs) are secondary plant metabolites witch can contaminate food, especially herbs. Due to the fact that alkaloids have a strong adverse effect on human health, it is necessary to use sensitive and selective detection methods. In present study a modified method based on LC-MS/MS was developed and validated for the simultaneous determination of thirty pyrrolizidine alkaloids and their corresponding N-oxides (PANOs) in herbs samples. Sample extraction was based on ultrasound-assisted dispersive solid phase extraction and clean-up using graphene. Method validation showed that the proposed method hold good recoveries (61-128 %) for PAs/PANOs with RSD <15 %. Limits of quantification has been set at 1 μg kg level for all targeted alkaloids. The optimized method yielded a small matrix effect (-20-20 %) for most PAs/PANOs. The uncertainty associated with the analytical method was not higher than 38 %. The method is operationally simple, time-saving, and can be applied to the analysis of real herb samples.
吡咯里西啶生物碱（PAs）是次生植物代谢物，可污染食物，特别是草药。由于生物碱对人体健康有很强的不良影响，因此有必要使用灵敏和选择性的检测方法。在本研究中，开发并验证了一种基于 LC-MS/MS 的改良方法，用于同时测定草药样品中的三十种吡咯里西啶生物碱及其相应的 N-氧化物（PANOs）。样品提取基于超声辅助分散固相萃取和使用石墨烯进行净化。方法验证表明，该方法对 PAs/PANOs 的回收率良好（61-128%），RSD<15%。所有目标生物碱的定量限均设定为 1μgkg 水平。该方法对大多数 PAs/PANOs 的基质效应较小（-20-20%）。与分析方法相关的不确定度不高于 38%。该方法操作简单，耗时短，可应用于实际草药样品的分析。
