超高效液相色谱-大气压化学电离-三重四极杆质谱联用法快速测定食品中苯并[a]芘

doi:10.3724/SP.J.1123.2017.02021

摘要/Abstract

摘要：

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。

关键词: 苯并[a]芘, 超高效液相色谱-串联质谱, 大气压化学电离, 分子印迹固相萃取, 食品

Abstract:

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.

Key words: atmospheric pressure chemical ionization (APCI), benzo[a]pyrene, food, molecularly imprinted solid-phase extraction (MIP-SPE), ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

中图分类号:

O658

张晓艺, 张秀尧, 蔡欣欣, 李瑞芬. 超高效液相色谱-大气压化学电离-三重四极杆质谱联用法快速测定食品中苯并[a]芘[J]. 色谱, 2017, 35(6): 608-612.

ZHANG Xiaoyi, ZHANG Xiuyao, CAI Xinxin, LI Ruifen. Rapid determination of benzo[a]pyrene in foods by ultra performance liquid chromatography-triple quadrupole mass spectrometry with atmospheric pressure chemical ionization[J]. Chinese Journal of Chromatography, 2017, 35(6): 608-612.

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