SPE-UPLC-MS/MS快速测定豆制品中的乌洛托品

建立了一种固相萃取-超高效液相色谱质谱联用(SPE-UPLC-MS/MS)测定豆制品中乌洛托品的分析方法。样品经粉碎后,采用乙腈提取,ProElut PXA小柱净化,Shim-pack XR-ODS色谱柱分离,在电喷雾正离子模式下用质谱仪进行MRM分析。结果表明:乌洛托品在0～160μg/kg范围内呈现良好的线性关系,线性相关系数为0.9998,该方法对应的检出限和定量限分别为0.3μg/kg和1μg/kg在5～100μg/kg添加水平下,乌洛托品回收率为88.4%～97.1%,相对标准偏差为5.39%～8.74%。该方法简便,快速,可成功应用于豆制品中乌洛托品的检测。

A rapid method for the determination of urotropine in soy products by SPE-UPLC-MS/MS

An efficient method of urotropinein soy products was developed bysolid extraction-ultra pressure high performanceliquid chromatography-mass spectrometry（SPE-UPLC-MS/MS）.The sample was firstly ground,extracted by acetonitrile,purified by ProElut PXA solid extraction column,then separated by Shim-pack XR-ODS column,and finally determined by mass spectrometry under multiple reaction monitoring（MRM） with positive electrospray ionization.The results indicated that urotropine can reach a good linear relationship within the concentration range of 0 to 160 ug/kg with R2=0.9998,and the limits of detection and quantification were 0.3μg/kg and 1μg/kg,respectively.The recoveries of the blank with the added level from 5 to100μg/kg were88.4%~97.1%,and RSD was5.39%~8.74%.The method developed in this study is easy to operate,andcan successfully applied in the fast determination of urotropinein soy products.