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超高效液相色谱-大气压化学电离三重四极杆质谱法快速测定食品中的苯并[]芘

[Rapid determination of benzo[]pyrene in foods by ultra performance liquid chromatography-triple quadrupole mass spectrometry with atmospheric pressure chemical ionization].

作者信息

Zhang Xiaoyi, Zhang Xiuyao, Cai Xinxin, Li Ruifen

机构信息

Wenzhou Municipal Center for Disease Control and Prevention, Wenzhou 325001, China.

出版信息

Se Pu. 2017 Jun 8;35(6):608-612. doi: 10.3724/SP.J.1123.2017.02021.

Abstract

A method for the determination of benzo[]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 -hexane after spiked with benzo[]pyrene-d, and purified using MIP-SPE to eliminate most of the coextracts. The separation of benzo[]pyrene was carried out on an XBridge BEH C 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[]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[]pyrene in food samples.

摘要

建立了一种基于同位素稀释和分子印迹固相萃取(MIP-SPE)的超高效液相色谱-串联质谱法(UPLC-MS/MS)测定食品中苯并[]芘的方法。样品中的目标分析物在加入苯并[]芘-d后用正己烷萃取,并用MIP-SPE纯化以去除大部分共提取物。苯并[]芘在XBridge BEH C柱上进行分离,采用甲醇和水梯度洗脱。使用大气压化学电离(APCI)接口作为离子源,在多反应监测(MRM)模式下进行分析。该方法可准确测定0.07-50μg/kg范围内的苯并[]芘含量,定量限(LOQ)为0.07μg/kg。平均回收率在86%至104%之间,相对标准偏差在2.3%-14%以内。该方法灵敏、准确,已成功应用于食品样品中苯并[]芘的测定。

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