title: Determination of aristolochic acid I in botanicals and dietary supplements potentially contaminated with aristolochic acid I using LC-UV with confirmation by LC/MS: collaborative study.
abstract: An interlaboratory study was conducted to evaluate a method for the determination of aristolochic acid I, also known as aristolochic acid A, at levels > 2.00 microg/g in botanical species and dietary supplements potentially contaminated with aristolochic acid I. Aristolochic acid I was extracted from various matrixes with aqueous acetonitrile. The amount of aristolochic acid I present was determined by liquid chromatography (LC) using an ultraviolet (UV) detector with confirmation by LC/mass spectrometry (MS). Thirteen blind duplicates were successfully analyzed by 10 collaborators, and aristolochic acid I was successfully confirmed in 1 blind duplicate by 8 collaborators. For repeatability, the relative standard deviation (RSD(r)) ranged from 1.72 to 16.3% and for reproducibility, the RSDR ranged from 5.42 to 19.8%. HorRat values were not applicable for 2 materials but varied from 0.7 to 1.8 for 11 materials. Each collaborating laboratory had calibration curves with correlation coefficients > 0.998. In addition, all of the collaborators that conducted the confirmation were able to verify the identity of aristolochic acid I using LC/MS/MS (using either ion trap or triple quad).
authors.affiliation: Covance Laboratories, 3301 Kinsman Blvd, Madison, WI 53704, USA. wendy.sorenson@covance.com
authors.forename: Wendy R
authors.initials: WR
authors.lastname: Sorenson
authors.forename: Darryl
authors.initials: D
authors.lastname: Sullivan
mesh_terms: D034341:Aristolochic Acids / Q000032:analysis*; D002138:Calibration; D002623:Chemistry Techniques, Analytical / Q000379:methods*; D002845:Chromatography; D002851:Chromatography, High Pressure Liquid; D002853:Chromatography, Liquid / Q000379:methods; D019587:Dietary Supplements / Q000032:analysis*; D004305:Dose-Response Relationship, Drug; D013058:Mass Spectrometry / Q000379:methods; D010936:Plant Extracts / Q000032:analysis*; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013056:Spectrophotometry, Ultraviolet / Q000379:methods; D013997:Time Factors
chemical_list: D034341:Aristolochic Acids; D010936:Plant Extracts; C000228:aristolochic acid I