基质分散固相萃取-UPLC-MS/MS测定烟草中马来酰肼残留量

Determination of maleic hydrazide residues in tobacco by with UPLC-MS/MS matrix dispersive solid phase extraction

建立了烟草中马来酰肼残留检测的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。烟叶样品经盐酸溶液回流萃取,氘代同位素内标定量,PSA净化和UPLC-MS/MS分析测定,分析时间仅需8 min。结果表明,马来酰肼的工作曲线在50 ng/mL~5000 ng/mL之间线性关系良好(R 2>0.99),各种烟叶基质中马来酰肼的检出限(LOD,以S/N=3计)范围为0.624~987 ng/mL;在2.5,15和100 ng/g加标水平下,加标回收率在105.9%~111.8%之间,RSD范围为3.3%~9.1%。本方法具有快速,简便,准确性好的特点,适用于烟草中马来酰肼残留量的检测。

Samples were extracted by HCl aqueous solution,with d 2-maleic hydrazide as the internal standard,purified by N-propylethane-1,2-dia mine(primary secondary amine,PSA),and finally detected by UPLC-MS/MS.It took only 8 minutes to complete the analysis.The results showed that the calibration curve of maleic hydrazide had good linearity in the range of 50—5000 ng/mL with R 2 higher than 0.99,the detection limits(LOD,S/N=3)of maleic hydrazide in various tobacco substrates ranged from 0.624 to 987 ng/mL.The recoveries ranged from 105.9%to 111.8%,and the RSD ranged from 3.3%to 9.1%at three spiked levels.This method is sensitive,accurate and fast.