Journal
FOOD ADDITIVES AND CONTAMINANTS PART A-CHEMISTRY ANALYSIS CONTROL EXPOSURE & RISK ASSESSMENT
Volume 31, Issue 5, Pages 784-791Publisher
TAYLOR & FRANCIS LTD
DOI: 10.1080/19440049.2014.892215
Keywords
aristolochic acid; herbal dietary supplements; LC-MS
Funding
- US Department of Energy
- US Food and Drug Administration
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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): 5/10ngg(-1) (tablets); 25/50ngg(-1) (capsules); and 2.5/5.0ngml(-l) (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.
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