Simultaneous Determination of Pyrrolidine Alkaloids and Their Nitrogen Oxides in Farfarae Flos by UPLC-MS/MS / 中国实验方剂学杂志

<b>Objective::To establish an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the simultaneous determination of 15 pyrrolidine alkaloids (PAs) and their nitrogen oxides, and determine the content of the 15 PAs in the 15 batches of Farfarae Flos samples obtained from different sources, in order to understand the distribution status of these 15 PAs in Farfarae Flos from different sources, and provide relevant references for the safe and rational use of this medicinal materials. <b>Method::The method was achieved by Agilent Eclipse Plus C₁₈ column (3.0 mm×150 mm, 1.8 μm) using a mobile phase made up of 0.05%formic acid and 2.5 mmol·L^-1 ammonium formate in water (A)-0.05%formic acid and 2.5 mmol·L^-1 ammonium formate in methanol(B). The flow rate and the injection volume were 0.4 mL·min^-1 and 2 μL, respectively. The column temperature was 40 ℃. The instrument was Agilent 1290-6470 QQQ ultra high performance liquid chromatography-triple quaternary bar mass spectrometer. The components were detected in multiple reaction monitoring mode by mass spectrometry with ionizationmode of ESI⁺. The content of the components measured in the samples was calculated by using the external standard method, and the difference between samples was analyzed based on RSD of different components. <b>Result::The established method had a high sensitivity and good separation degree. The results of methodological investigation met the requirements. The results showed that all of the 15 batches of Farfarae Flos contained PAs and their nitrogen oxides. These PAs had almost the same types of structure. There were significant differences in the content and distribution of PAs in Farfarae Flos obtained from different sources. <b>Conclusion::In general, Farfarae Flos contains pyrrolidine alkaloids and their nitrogen oxides. Senkirkine with a significant hepatotoxicity is the main compound. The content determination of PAs will provide scientific fundaments for the safe and effective use of Farfarae Flos.

Isolation and Elucidation of Pyrrolizidine alkaloids from tuber of Gynura pseudo-china (L.) DC.

Pyrrolizidine alkaloids (PAs) are produced by numerous plant species throughout the world. Numerous intoxications in animals and humans caused by the consumption of certain plants were attributed from the middle of this century to compounds of vegetable origin, the pyrrolizidine alkaloids. Daun dewa (Gynura pseudo-china (L.) DC.) is one of Indonesian medicinal plant which also a native plant of India, Thailand and China. The tuber of this plant is commonly used in Indonesian traditional medicine such as for treatments of uterine hemorrhages, dysentery, and inflamed wounds. Although its medicinal value, it is reported that leaves of this plant and other Gynura species content pyrrolizidine alkaloids (PAs). There are concern about the present of PAs in medicinal plants because of the toxicity of this compounds to human and animal. It is reported that PAs are hepatotoxic, pneumotoxic, genotoxic, neurotoxic, and cytotoxic. The purpose of this study is to study the PAs content of G. pseudochina tuber. The structures-were elucidated using spectral data of Infra Red, Liquid Chromatography-Mass Spectroscopy and a combination of one- and two dimensional 1H and 13C- Nuclear Magnetic Resonance spectroscopy. In this study, two pyrrolizidine alkaloids, senecionine (Compound 1) and senkirkine (Compound 2) were isolated from the tuber of G. pseudo-china. This results suggest that it should be a safety consideration in consuming this plant for traditional medicine because it is also contains PAs which are toxic compounds.