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    在线液相-气相二维色谱-质谱联用法测定烟用香精和料液中苯并a芘的含量

    Determination of Benzoapyrene in Tobacco Flavour and Liquid Stuff by On-line 2-Dimensional Liquid-Gas Chromatography in Hyphenation with Mass Spectrometry

    • 摘要: 样品10.0 g,加水10 mL稀释,加0.100 g·L-1 D12-苯并a芘内标溶液200 μL,加环己烷10 mL,以20 000 r·min-1速率漩涡振荡萃取5 min。提取液直接进入液相色谱,经微型硅胶柱分离净化,含苯并a芘的部位切割进入气相色谱,经毛细管柱分离后进入质谱分析,采用选择离子监测模式(SIM)进行测定。苯并a芘的质量浓度在0.08~50 ng·L-1范围内与峰面积呈线性关系,方法的检出限(3s)为0.12 ng·g-1,在3个不同浓度水平上进行了回收试验,回收率在92.7%~98.1%之间,测定值的相对标准偏差(n=7)在3.2%~3.7%之间。

       

      Abstract: The sample (10.0 g) was diluted with 10 mL of water, and 200 μL of 0.100 g·L-1 BaP-D12 solution were added as internal standard. The solution was then extracted with 10 mL of cyclohexane by vortical oscillation for 5 min at a rate of 20 000 r·min-1. The extract was separated and purified by HPLC through direct injection into the silica gel micro-column. The part with BaP structure was cut and transferred into GC, and separated on capillary column. SIM was adopted in MS. Linear relationship between values of peak area and mass concentration of BaP was found in the range of 0.08-50 ng·L-1, with detection limit (3s) of 0.12 ng·g-1. Values of recovery found by standard addition method at 3 concentration levels were in the range of 92.7%-98.1%, with RSDs (n=7) in the range of 3.2%-3.7%.

       

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