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目的建立气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)测定食用植物油中苯并(α)芘的分析方法。方法用石油醚提取食用植物油样品,经过中性氧化铝柱净化,再用石油醚洗脱,最后经过氮吹来浓缩定容。然后采用三重四级杆气质联用仪多重反应监测(multiple reaction monitor,MRM)模式进行测定,随后对质谱测定的目标离子对进行选择。结果苯并(α)芘的质量浓度为0.1~20μg/L范围时,其峰面积与浓度间呈现良好的线性关系,方法的定量限为1.0μg/kg,3个添加水平下(1.0、5.0和10.0μg/kg)的平均加标回收率为89.7%~117.8%,相对标准偏差在3.2%~9.0%之间。结论本方法精密度和准确度较好,能够实现植物油样品中苯并(α)芘的准确测定。
Objective To establish a method for the determination of benzo (α) pyrene in edible vegetable oils by gas chromatography-tandem mass spectrometry (GC-MS / MS). Methods Samples of edible vegetable oil were extracted with petroleum ether, purified by a neutral alumina column, eluted with petroleum ether, and finally concentrated by nitrogen. The assay is then performed using a triple quadrupole multiplex reaction monitor (MRM) mode, followed by the selection of the target ion pair for mass spectrometry. Results When the mass concentration of benzo (α) pyrene was in the range of 0.1 ~ 20μg / L, the linear relationship between peak area and concentration was obtained. The limit of quantification was 1.0μg / kg. Under the three addition levels And 10.0μg / kg) were 89.7% ~ 117.8%, the relative standard deviations were between 3.2% ~ 9.0%. Conclusion The method has good precision and accuracy, and can accurately determine benzo (α) pyrene in vegetable oil samples.