Vaclavik Lukas, Krynitsky Alexander J, Rader Jeanne I
a Center for Food Safety and Applied Nutrition, Office of Regulatory Science , US Food and Drug Administration , College Park , MD , USA.
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.
建立并评估了一种快速、选择性和灵敏的超高效液相色谱-多级碎裂质谱法（UHPLC-MS³），用于测定草药膳食补充剂中的马兜铃酸I和II（AA I和II）。采用混合三重四极杆/线性离子阱质谱监测MS³离子跃迁m/z 359.2 > 298.1 > 268.0和m/z 329.2 > 268.2 > 238.0，分别检测AA I和II。使用快速简便、价廉、高效、耐用且安全（QuEChERS）的方法从干粉状样品中提取和净化目标分析物。直接分析草药液体提取物。平均回收率为89%至112%，相对标准偏差（RSD）为3%至16%。对三种选定基质估计的定量限（LOQ）如下（AA I/II）：5/10 ng g⁻¹（片剂）；25/50 ng g⁻¹（胶囊）；以及2.5/5.0 ng ml⁻¹（草药液体提取物）。该方法应用于对30种通过互联网在美国销售的草药产品的有限调查。在所测试的样品中，分别有20%和7%检测到了AA I和II。
