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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

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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 g/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 (RSDr) 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).

Document Type: Research Article

Affiliations: Covance Laboratories, 3301 Kinsman Blvd, Madison, WI 53704.

Publication date: July 1, 2007

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  • The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
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