Quantification of aristolochic acids I and II in herbal dietary supplements by ultra-high-performance liquid chromatography-multistage fragmentation mass spectrometry

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2014;31(5):784-91. doi: 10.1080/19440049.2014.892215. Epub 2014 Apr 8.


A rapid, selective and sensitive ultra-high-performance liquid chromatography-multistage fragmentation mass spectrometry (UHPLC-MS³) method was developed and evaluated for the determination of aristolochic acids I and II (AA I and II) in herbal dietary supplements. A hybrid triple quadrupole/linear ion-trap mass spectrometry was used to monitor MS³ ion transitions m/z 359.2 > 298.1 > 268.0 and m/z 329.2 > 268.2 > 238.0 to detect AA I and II, respectively. The extraction and clean-up of target analytes from dry powdered samples was performed using the quick, easy, cheap, effective, rugged and safe (QuEChERS) procedure. Herbal liquid extracts were analysed directly. Average recoveries ranged from 89% to 112%, with relative standard deviations (RSDs) ranging from 3% to 16%. Limits of quantification (LOQs) estimated for three selected matrices were as follows (AA I/II): 5/10 ng g⁻¹ (tablets); 25/50 ng g⁻¹ (capsules); and 2.5/5.0 ng ml⁻¹ (liquid herbal extract). The method was applied in a limited survey of 30 herbal products marketed in the United States via the Internet. AA I and II were detected in 20% and 7%, respectively, of tested samples.

Keywords: LC-MS; aristolochic acid; herbal dietary supplements.

Publication types

  • Evaluation Study
  • Research Support, U.S. Gov't, Non-P.H.S.

MeSH terms

  • Analytic Sample Preparation Methods
  • Aristolochic Acids / analysis*
  • Aristolochic Acids / chemistry
  • Carcinogens / analysis*
  • Carcinogens / chemistry
  • Chromatography, High Pressure Liquid
  • Dietary Supplements / analysis*
  • Dietary Supplements / economics
  • Drug Contamination
  • Drugs, Chinese Herbal / chemistry
  • Drugs, Chinese Herbal / economics
  • Food Contamination*
  • Food Inspection / methods*
  • Internet
  • Limit of Detection
  • Plant Extracts / chemistry
  • Plant Extracts / economics
  • Plant Preparations / chemistry*
  • Plant Preparations / economics
  • Poisons / analysis
  • Poisons / chemistry
  • Reproducibility of Results
  • Spectrometry, Mass, Electrospray Ionization
  • Tandem Mass Spectrometry
  • United States


  • Aristolochic Acids
  • Carcinogens
  • Drugs, Chinese Herbal
  • Plant Extracts
  • Plant Preparations
  • Poisons
  • aristolochic acid I
  • aristolochic acid II