title: Quantification of aristolochic acids I and II in herbal dietary supplements by ultra-high-performance liquid chromatography-multistage fragmentation mass spectrometry.
abstract: 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.
authors: a Center for Food Safety and Applied Nutrition, Office of Regulatory Science , US Food and Drug Administration , College Park , MD , USA.
authors: Lukas
authors: L
authors: Vaclavik
authors: Alexander J
authors: AJ
authors: Krynitsky
authors: Jeanne I
authors: JI
authors: Rader
mesh_terms: D053000:Analytic Sample Preparation Methods; D034341:Aristolochic Acids / Q000032:analysis* / Q000737:chemistry; D002273:Carcinogens / Q000032:analysis* / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid; D019587:Dietary Supplements / Q000032:analysis* / Q000191:economics; D004340:Drug Contamination; D004365:Drugs, Chinese Herbal / Q000737:chemistry / Q000191:economics; D005506:Food Contamination; D005513:Food Inspection / Q000379:methods*; D020407:Internet; D057230:Limit of Detection; D010936:Plant Extracts / Q000737:chemistry / Q000191:economics; D028321:Plant Preparations / Q000737:chemistry* / Q000191:economics; D011042:Poisons / Q000032:analysis / Q000737:chemistry; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization; D053719:Tandem Mass Spectrometry; D014481:United States
chemical_list: D034341:Aristolochic Acids; D002273:Carcinogens; D004365:Drugs, Chinese Herbal; D010936:Plant Extracts; D028321:Plant Preparations; D011042:Poisons; C000228:aristolochic acid I; C042310:aristolochic acid II
keywords: LC-MS; aristolochic acid; herbal dietary supplements