建立了快速检测食品中苯并[a]芘的超高效液相色谱-三重四极杆质谱联用(UPLC-MS/MS)分析方法.样品用正己烷提取后,经分子印迹固相萃取柱净化,以甲醇和水作为流动相进行梯度洗脱,在XBridge BEH C18柱上实现分离,大气压化学电离(APCI)-三重四极杆质谱正离子MRM方式检测,以苯并[a]芘-d12作为内标的稳定同位素稀释法定量.方法的线性范围为0.07~50 μg/kg,定量限为0.07 μg/kg.平均加标回收率为86%~104%,相对标准偏差为2.3%~14%.该方法灵敏、准确,适用于食品中苯并[a]芘的测定,已应用于实际样品的检查.
A method for the determination of benzo[a]pyrene in foods was developed by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) based on isotope dilution and molecularly imprinted solid-phase extraction (MIP-SPE).The target analyte in samples was extracted with n-hexane after spiked with benzo[a]pyrene-d12,and purified using MIP-SPE to eliminate most of the coextracts.The separation of benzo[a]pyrene was carried out on an XBridge BEH C18 column with gradient elution of methanol and water.An atmospheric pressure chemical ionization (APCI) interface was used as the ion source and the analysis was performed in the multiple reaction monitoring (MRM) mode.Benzo[a]pyrene levels in the range of 0.07-50 μg/kg were measured accurately by this method,and the limit of quantification (LOQ) was 0.07 μg/kg.The average recoveries were between 86% and 104% with the relative standard deviations within 2.3%-14%.The method was sensitive and accurate,and it has been successfully applied to the measurement of benzo[a]pyrene in food samples.
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