Simultaneous determination of 7 pyrrolizidine alkaloids and their nitrogen oxides in herbal tea by SPE-UPLC-MS/MS
A analysis method for simultaneous determination of 7 pyrrolizidine alkaloids and their nitrogen oxides(monocrotaline,monocrotaline N-oxide,lycopsamine,lycopsamine-N-oxide,heliosinine,heliosinine-N-oxide,senecionine)in herbal tea was established by solid phase extraction-ultra high performance liquid chromatography tandem mass spectrometry(SPE-UPLC-MS/MS).The samples were extracted by 0.1 mol/L hydrochloric acid solution and purified by MCX solid phase extraction column,separated by Poroshell 120 EC-C18 chromatographic column(150 mm×3.0 mm,2.7 μm),and detected by electrospray positive ionization multiple reaction monitoring(MRM)mode.The results showed that the 7 pyrrolizidine alkaloids and their nitrogen oxides showed good linear relationships in the linear range of 1.0-50 μg/L,and the correlation coefficients(R2)were both greater than 0.998.The limits of detection(LOD)and limits of quantitation(LOQ)were 0.3 μg/kg and 1.0 μg/kg,respectively.Average spiked recovery rates were 81.8％-9 8.8％,and the relative standard deviations(RSD)of precision experiment results were 1.98％-7.08％.The results of 20 herbal tea samples tested were found that 2 samples were detected with senecionine,which were 18.2 μg/kg and 33.5 μg/kg,respectively.The method was rapid,accurate,ac-curate and suitable for simultaneous determination of pyrrolizidine alkaloids and their nitrogen oxides in herbal tea.
ultra high liquid chromatography tandem mass spectrometrysolid phase extractionherbal teapyrrolizidine alkaloidsnitrogen oxide
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