UPLC-MS/MS法同时测定地沟油中特征组分

Simultaneous Determination of Characteristic Components in Hogwash Oil Using UPLC-MS/MS

应用超高效液相色谱-串联质谱联法（UPLC-MS/MS）建立了地沟油中辣椒碱、二氢辣椒碱、合成辣椒碱和胡椒碱4种特征组分的分析方法。通过对固相萃取柱、淋洗液和流动相等的优化,确定以Oasis HLB固相萃取柱、乙腈为淋洗液、水（0.1%甲酸）-乙腈（7∶3,V/V）为流动相做样品预处理。在最优条件下,目标物的回收率均85.5%-108.3%,相对标准偏差（RSDs）在7.8%-10.6%,线性范围均在1-2 000μg/L,各目标物标准品在UPLC-MS/MS系统中有效的线性相关（R2）为0.999以上。该方法具有检测限低、回收率高等优点,经实际样品测试,可用于地沟油中辣椒碱等4种特征组分的同时检测。

An analytical method for simultaneous determination of characteristic components in hogwash oil samples was developed by solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometer （UPLC-MS/ MS）. An Oasis HLB solid phase extraction column, acetonitrile as washing solution and water （0.1% formic acid）-acetonitrile （7 ： 3, V/V） as the mobile phases, was selected for sample pretreatment and chromatographic separation. Based on the optimized sample pretreatment procedures and separation condition, the target recoveries ranged from 85.5% to 108.3% with the relative standard deviations （RSDs） from 7.8% to 10.6%, the linear ranged from 1 to 2 000 μg/L with correlation coefficients （R2） no less than 0.999. The method could be applied to simultaneous determination of 4 characteristic components in hogwash oil samples because of its low detection limits and high recoveries.