Determination of Pyrrolizidine Alkaloids in Dendrobium officinale Kimura et Migo by UPLC-MS/MS
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Abstract:
In order to determine the content of pyrrolizidine alkaloids (PAs) in Dendrobium officinale Kimura et Migo, an analytical method for the simultaneous determination of 16 kinds of unsaturated PAs in Dendrobium officinale Kimura et Migo by solid phase extraction combined with ultra performance liquid chromatography-tandem mass spectrometry was established in this study. Samples were extracted with 0.05 mol/L sulfuric acid methanol, purified and enriched by MCX solid-phase extraction cartridge. The mobile phases were methanol and 0.005 mol/L of ammonium formate - 0.1% of formic acid solution. The separation was performed on a Waters ACQUITY UPLC BEH C18 column with gradient elution. The electrospray positive ion and multi-reaction monitoring mode were used for acquisition, and matrix matching external standard method was used for quantification. The results showed that the linear range of 16 kinds of PAs in this method was 0.5~20 μg/L, and the correlation coefficients were all greater than 0.99. The limits of detection were 0.06~0.11 μg/kg, and the limits of quantification were 0.23~0.35 μg/kg. At the spiked levels of 0.5, 1.0 and 10 μg/kg, the average recoveries ranged from 75.38% to 110.27%, with the relative standard deviations ranging from 2.61% to 7.43%. This method was used to determine the PAs in 20 Dendrobium officinale Kimura et Migo samples commercially available. The results showed that 7-acetyllycopsamine was detected in 12 samples with the content ranging from 1.02~6.54 μg/kg. The method is simple, sensitive and accurate, and is suitable for rapid confirmation and quantitative analysis of PAS in Dendrobium officinale Kimura et Migo.
