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气相色谱-质谱法测定烟草中多氯联苯

Determination of PCBs in tobacco by GC/MS

  • 摘要: 为加强口含烟烟叶原料外源性污染风险管控,对烟叶中可能含有的多氯联苯(PCBs)的定性定量检测方法进行了研究,建立了同时检测烟草中7种指示性PCBs的气相色谱-质谱方法,并对国内外42个片烟样品进行了检测。烟末样品经萃取、真空浓缩、二次溶解净化后,直接用气质联用仪在选择离子监测模式下检测,采用内标法定量。结果表明:① 7种PCBs的浓度/响应值关系拟合曲线线性良好,R2在0.984 3~0.994 8之间。② 在优化条件下,7种PCBs的检出限和定量限分别为0.22~1.07和0.73~3.57 ng· mL-1,样品加标回收率为70.4%~95.5%,日内和日间相对标准偏差分别≤ 4.6%和9.2%。③ 7种PCBs在42个样品中有不同程度的检出,总量最高为0.37 mg·kg-1,均低于食品中PCBs的限量标准(总量≤0.5 mg·kg-1)。该方法简单、快速,适用于烟草样品中PCBs的检测。

     

    Abstract: In order to control exogenous contamination risks for raw materials used in oral tobacco products, a qualitative and quantitative analysis method for polychlorinated biphenyls(PCBs)in tobacco leaves was established. The developed method for the simultaneous determination of seven PCBs in tobacco by gas chromatography-mass spectrometry(GC-MS)was applied to test 42 domestic and imported tobacco samples. After extraction, vacuum concentration to drying, re-dissolving and purification, the tobacco powder samples were quantified by gas chromatography-mass spectrometry(GC-MS) with internal standards. The results showed that:1) The linearity of curves of the seven PCBs'concentration-response relationship was good with the correlation coefficient range between 0.984 3-0.994 8. 2) The limit of detection and the limit of quantification were 0.22-1.07 and 0.73-3.57 ng·mL-1, respectively. The spiked recovery ranged from 70.4% to 95.5% with the intra-day and inter-day relative standard deviations no more than 4.6% and 9.2%, respectively. 3) Different amounts of the seven PCBs were detected in the 42 samples with the maximum total amount of 0.37 mg·kg-1, which was lower than the limit level of PCBs in food(≤ 0.5 mg·kg-1 in total). This method is simple, rapid and suitable for the detection of PCBs in tobacco samples.

     

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