超高效液相色谱-串联质谱法测定铁皮石斛中的吡咯里西啶生物碱

为了测定铁皮石斛中的吡咯里西啶生物碱(pyrrolizidine alkaloids,PAs)的含量,该研究建立了固相萃取结合超高效液相色谱-串联质谱法同时测定铁皮石斛中16种不饱和PAs的分析方法.样品经0.05 mol/L硫酸甲醇提取、MCX固相萃取小柱纯化富集,以甲醇和0.005 mol/L甲酸铵-0.1％甲酸水...

Determination of Pyrrolizidine Alkaloids in Dendrobium officinale Kimura et Migo by UPLC-MS/MS

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 0.5~20μg/L,and the correlation coefficients were all greater than 0.99.The limits of detection were 0.06~0.11μg/kg,and the limits of quantification were 0.23~0.35μg/kg.At the spiked levels of 0.5,1.0 and 10μg/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 1.02~6.54μg/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.