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Abstract: LC/(+)ESI/MS3 was used to determine aconitine, mesaconitine, and hypaconitine as target markers in crude methanol extracts of (i) the raw lateral roots of Aconitum carmichaeli, (ii) roots treated by three different refining processes, and (iii) eight generally available traditional Chinese medicine (TCM) preparations containing fuzi (treated lateral roots of A. carmichaeli). The optimal ionization behavior resulted when using electrospray ionization (ESI) in positive-ion mode with 0.005% TFA as an additive in the mobile phase. The consecutive reaction monitoring (CRM) mode provided additional improvements in selectivity, which was exploited to minimize the noise and interference problems. Employing this approach, aconitine and mesaconitine were found to decompose readily during the refining processes, but hypaconitine remains present at the same content, presumably because of its characteristic chemical structure. Thus, treated and untreated fuzi samples can be distinguished by monitoring the ratio of aconitine and mesaconitine to hypaconitine. The limits of detection (LODs) for these three markers were 0.05, 0.08, and 0.03ng/ml. The linearity range for the three marker compounds was 0.1–1000ng/ml. The analysis time was 12min per sample. [Copyright &y& Elsevier]

In this study, five flavonoid glycosides were extracted from defatted Camellia oleifera seeds by using a pressurized hot water extraction (PHWE) method. The independent experimental factors (temperature, time and pressure) influencing the PHWE efficiency of the flavonoid glycosides were optimized and quantified using an orthogonal array design and high-performance liquid chromatography – negative mode electron spray ionization/mass spectrometry (HPLC/(−)ESI–MS-MS), respectively. Based on the result of experimental design, the maximum extraction efficiency of flavonoid glycosides were obtained by selecting temperature at 140 °C, pressure at 600 psi, and time for 10 min. The recovery and overall yield of the flavonoid glycosides were greater than those in ultrasonic extraction (UE) (78.5% vs 68.4% and 18.8 mg/g vs 15.91 mg/g). In particularly, compounds 1 and 2, which are kaempferol derivatives, were higher 1.19–1.23 times than those of the compounds obtained through UE (6.63 mg/g vs 5.56 mg/g; 11.89 mg/g vs 9.66 mg/g, respectively). These two compounds have higher polarities and antioxidant capacities than the other three flavonoid glycosides. Thus, PHWE is an excellent alternative method for the extraction of flavonoid glycosides that are highly polar and potent antioxidants. [ABSTRACT FROM AUTHOR]