A novel approach for fast and simple determination pyrrolizidine alkaloids in herbs by ultrasound-assisted dispersive solid phase extraction method coupled to liquid chromatography-tandem mass spectrometry

J Pharm Biomed Anal. 2020 Aug 5:187:113351. doi: 10.1016/j.jpba.2020.113351. Epub 2020 May 5.

Abstract

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-1 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.

Keywords: Dispersive solid phase extraction; Herbs; LC–MS/MS; Pyrrolizidine alkaloids; Ultrasound-assisted.

Publication types

  • Validation Study

MeSH terms

  • Chromatography, Liquid / methods*
  • Limit of Detection
  • Oxides / analysis
  • Oxides / isolation & purification
  • Plant Extracts / analysis*
  • Plant Extracts / chemistry
  • Pyrrolizidine Alkaloids / analysis*
  • Pyrrolizidine Alkaloids / isolation & purification
  • Solid Phase Extraction
  • Tandem Mass Spectrometry / methods*
  • Ultrasonic Waves

Substances

  • Oxides
  • Plant Extracts
  • Pyrrolizidine Alkaloids