通过优化食用植物油前处理方法,建立一种QuEChERS-同位素内标-超高效液相色谱-串联质谱法测定食用植物油中乙基麦芽酚含量。样品经水-甲醇提取后,采用十八烷基键合硅胶(C18)和 N-丙基乙二胺 (PSA)净化,通过Waters HSS T3色谱柱分离,多反应监测(MRM)模式监测,内标法定量。研究结果表明,乙基麦芽酚在2 ng/mL-100 ng/mL范围内具有良好的线性关系,检出限为10.0 μg/kg,定量限为 25.0 μg/kg,在3个加标水平下的平均回收率为78.1%-101.7%,批内精密度为0.57%-4.44%。本方法具有操作简单、灵敏度和准确度高等特点,适用于大批量食用植物油样品中乙基麦芽酚含量的检测。
This study optimized the pretreatment method of edible vegetable oil and developed the analytical method for the determination of ethyl maltol in edible vegetable oil using ultra- performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)combined with QuEChERS-isotope internal standard. Samples were extracted with water-methanol, purified with octadecyl bonded silica gel (C18), N-propylethylenediamine (PSA). The extracts were chromatographically separated using a Waters HSS T3 column, followed by MS detection in multiple reaction monitoring (MRM) mode and quantified by internal standard method. Under optimized conditions, good linearity was observed for the ethyl maltol in the range of 2-100 ng/mL. The limits of detection and the limits of quantitation were 10.0 μg/kg and 25.0μg/kg, respectively. Average recoveries at three spiked levels ranged from 78.1% to 101.7%, with relative standard deviations (RSDs) of 0.57% to 4.44% (inter-batch, n=6). This method is fast, high sensitivity and accuracy, and suitable for determination of ethyl maltol in edible vegetable oil.