GC-MS/MS法检测山茶油中的苯并[α]芘

Determination of Benzo[α]pyrene in Camellia Oil by Gas Chromatography Tandem Mass Spectrometry

建立了山茶油中苯并[α]芘含量的液液萃取-气相色谱-三重串联四极杆质谱(GC-MS/MS)的检测方法。样品称量后加入苯并[a]芘-d12同位素内标,采用乙腈提取两次提取,正己烷脱脂净化后,气相色谱-三重串联四极杆质谱分析。采用DB 5-MS毛细管柱分离,串联四级杆质谱多反应监测模式检测,内标法定量。在优化实验条件下,苯并[α]芘的峰面积与其浓度在0.50μg/L-100μg/L范围内呈良好的线性关系,线性回归系数为0.9994,方法的检出限(LODs)为0.25μg/kg,定量限(LOQs)为0.50μg/kg,在加标水平为0.50、1.00、5.00μg/kg时,山茶油样品中苯并[α]芘的平均回收率在92.51-103.70%之间,日内分析的相对标准偏差(RSD,n=6)为3.84-5.80%,日间回收率为94.71-110.83%,相对偏差为5.22-8.92%(n=5)。该方法具有前处理简单、定量准确、灵敏度高的特点,适用于山茶油中苯并[α]芘的快速确认和准确定量。

A method was developed for the determining of benzo[α]pyrene in camellia oil by gas chromatography by tandem mass spectrometry（GC-MS/MS） with liquid-liquid extraction.After spiked with the isotopic labeled benzo[a]pyrene-d12,the sample was extracted twice with acetonitrile,and then defatted by n-hexane to obtain an extract suitable for analysis using GC-MS/MS.The targeted compound was separated by a DB 5-MS column detected by GC-MS/MS system under the mode of multiple reaction monitoring（MRM）.The internal standard was used for quantitative analysis.Under the optional conditions,the linear range was between 0.50 μg/L and 100 μg/L with the linear correlation coefficients of 0.9994.The detection limit of the method（LOD） was 0.25 μg/kg and the quantitation limit of the method（LOQ） was 0.5 μg/kg.The mean recoveries for camellia oil at three spiked concentrations levels of 0.50,1.00,5.00 μg/kg were ranged from 92.51% to 103.70%,respectively,with relative standard deviations（RSDs,n=6） 3.84-5.80%.The inter-recoveries were ranged from 94.71%-110.83% and the precision was ranged from 5.22% to 8.92%（n=5）.This method was suitable for the identification and quantification of benzo[α]pyrene in camellia oil due to its simplicity,accuracy and high sensitivity.