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作 者:王立云 陈莉莎 芦楠[1] 蒋成勇[1] 林琳 严莉红 WANG Liyun;CHEN Lisha;LU Nan;JIANG Chengyong;LIN Lin;YAN Lihong(Beijing Research Station of Technical Center,Shanghai Tobacco Group Co.,Ltd.,Beijing 101121,China;Beijing Tobacco Quality Control & Supervision Station,Beijing 100029,China)
机构地区:[1]上海烟草集团有限责任公司技术中心北京工作站,北京101121 [2]北京市烟草质量监督检测站,北京100029
出 处:《轻工学报》2019年第3期60-67,共8页Journal of Light Industry
摘 要:以极性DB-WAX毛细管柱为色谱柱、正己烷为萃取溶剂、正十四烷为内标物,建立了利用气相色谱-串联质谱仪(GC-MS/MS)同时测定烟用水基胶中的苯系物和邻苯二甲酸酯类化合物含量的方法,并对该方法的性能进行了考察.结果表明:在萃取时间为20 min时,采用MRM模式和最佳碰撞能量条件,实现了苯系物和邻苯二甲酸酯类化合物13种组分的完全分离.该方法的相关系数>0.999,苯系物的检出限为0.000 8~0.001 0 μg/mL,定量限为 0.002 5~ 0.003 0 μg/mL;邻苯二甲酸酯类化合物的检出限为0.003 0~ 0.008 0 μg/mL ,定量限为0.010 0~0.030 0 μg/mL;两类化合物各加标浓度水平下的回收率为83.2%~99.8%,相对标准偏差小于7.00%.这说明该方法重复性好,回收率高,可满足定量分析要求,且定量限低于行业标准.Using a polar DB-WAX capillary column as the column, n-hexane as the extract, and n-tetradecane as the internal standard, the simultaneous determination of the waterborne adhesives by gas chromatography-tandem mass spectrometry (GC-MS/MS) was established. The method for the content of benzene series and phthalate compounds was investigated and the performance of the method was examined. The results showed that the complete separation of 13 components of benzene series and phthalate compounds was achieved by MRM mode and optimal collision energy conditions at the optimum extraction time of 20 min. The correlation coefficient of this method was >0.999, the detection limit of benzene series was 0.000 8~0.001 0 μg/mL, the limit of quantification was 0.002 5~0.003 0 μg/mL;the detection limit of phthalate compounds was 0.003 0~ 0.008 0 μg/mL, the limit of quantification was 0.010 0~0.030 0 μg/mL;the recoveries of the two classes of compounds at each spiked concentration level were between 83.2%~99.8%, and the relative standard deviation was less than 7.00%. This indicated that the method had good repeatability and high recovery rate, which could meet the requirements of quantitative analysis, and the limit of quantitation was lower than the industry standard.
关 键 词:烟用水基胶 GC-MS/MS 苯系物 邻苯二甲酸酯类化合物
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