Rapid Determination of Aconitum Alkaloids from Human Urine by UHPLC–HRMS

: Aconitum alkaloid poisoning is a type of poisoning caused by accidental ingestion and clinical use of herbal drugs in many countries. In this study, we developed an in-syringe dispersive micro solid-phase extraction (DMSPE) method for selective extraction of aconitine, benzoylaconine and aconine from human urine using a type of polymer material. All of the parameters influencing the extraction efficiency such as the type and amount of sorbent, the extraction time and the desorption solvent and volume in DMSPE were carefully investigated and optimized. Using DMSPE method, the absence of evaporation and centrifugation steps reduced the consuming time of sample preparation. Samples were analyzed by ultra high-performance liquid chromatography-high-resolution mass spectrometry on an HSS T3 analytical column. The results showed that the DMSPE method yielded fewer relative and absolute matrix effects, which reduced the sample to sample variability in human urine. The limits of detection and limits of quantitation of this method were determined to be 0.08-0.1 and 0.2-0.3 μg/L, respectively. The average recoveries of the analytes were between 88.6% and 107.2% with the intra- and interday precisions ranging from 2.1% to 6.4% and from 5.9% to 13.9%, respectively. The method presented here is an efficient, low-cost and selective extraction of aconitine, benzoylaconine and aconine from human urine.