Background Pyrrolizidine alkaloids (PAs) are naturally occurring plant toxins associated with potential hepatic and carcinogenic diseases in humans and animals. The concern over PAs has increased as the consumption of herbal medicines has increased. Objective This study aimed to develop and validate a sensitive analytical method to determine 28 PAs in five herbal medicines using liquid chromatography (LC)-electrospray ionization (ESI)-tandem mass spectrometry (MS/MS). Additionally, this study identified and quantified the amount of PAs in 10 samples of each herbal medicine. Methods The pretreatment in the proposed LC-MS/MS analysis comprised solvent extraction using 0.05M H2SO4 in 50% methanol and clean-up step using an mixed-mode cationic exchange (MCX)-solid-phase extraction (SPE) cartridge. The PA contents in herbal medicines were measured by using the developed method. Results The proposed method had recoveries ranging from 72.5–123.7% for the Atractylodis Rhizoma Alba, 70.6–151.7% for Alba Chrysanthmi Flos, 80.6–130.9% for Leonuri Herba, 70.3–122.9% for Gastrodiae Rhizoma, and 67.1–106.9% for Glycyrrhizae Radix. Even though a few samples showed recoveries in unsatisfactory values, the proposed method indicated entirely sufficient recoveries and precision in most samples. In monitoring results, only Leonuri Herba contained two PAs, which indicated Retrorsine (4/10) of 84.7–120.9 μg/kg and Senkirkine (10/10) of 60.9–170.7 μg/kg. Conclusion The results obtained from this study demonstrate that the proposed method is fit for purpose to determine 28 PAs in herbal medicines. Therefore it could serve as a regulatory method capable of being used for controlling the risks of PAs in certain medicinal plants and dietary supplements. Highlights An LC-MS/MS method for the determination of 28 pyrrolizidine alkaloids in herbal medicines was developed and validated through this study. The proposed method is considered as an useful method for monitoring pyroolizidine alkaloids in herbal medicines.

中文翻译：

---

LC-ESI-MS/MS联用阳离子交换固相萃取测定五种中草药中吡咯里西啶生物碱

背景 吡咯里西啶生物碱 (PA) 是天然存在的植物毒素，与人类和动物的潜在肝脏和致癌疾病有关。随着草药消费量的增加，对 PA 的关注也有所增加。目的 本研究旨在开发和验证一种灵敏的分析方法，使用液相色谱 (LC)-电喷雾电离 (ESI)-串联质谱 (MS/MS) 测定五种草药中的 28 种 PA。此外，本研究确定并量化了每种草药的 10 个样本中的 PA 含量。方法 所提出的 LC-MS/MS 分析中的预处理包括使用 0.05M H2SO4 在 50% 甲醇中的溶剂萃取和使用混合模式阳离子交换 (MCX)-固相萃取 (SPE) 小柱的净化步骤。使用开发的方法测量草药中的 PA 含量。结果 所提出的方法对白术的回收率为 72.5-123.7%，白术为 70.6-151.7%，益母草为 80.6-130.9%，天麻为 70.3-122.9%，甘草为 67.1-106.9%基数。尽管少数样品的回收率值不令人满意，但所提出的方法在大多数样品中显示出完全足够的回收率和精密度。在监测结果中，只有益母草含有两种 PA，表明 Retrorsine (4/10) 为 84.7–120.9 μg/kg 和 Senkirkine (10/10) 为 60.9–170.7 μg/kg。结论 从本研究中获得的结果表明，所提出的方法适用于测定草药中的 28 种 PA。因此，它可以作为一种监管方法，用于控制某些药用植物和膳食补充剂中 PAs 的风险。亮点 通过本研究开发并验证了一种用于测定草药中 28 种吡咯里西啶生物碱的 LC-MS/MS 方法。所提出的方法被认为是监测草药中吡咯里西啶生物碱的有用方法。