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0.50 μg/L~100 μg/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0.25 μg/kg，定量限(LOQs)为0.50 μg/kg，在加标水平为0.50、1.00、5.00 μg/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.

广东省自然科学基金资助项目（S2011040004201）