基于顶空-气相色谱/质谱技术分析测定烟标印刷光油中挥发性有机化合物

Analysis and Determination of Volatile Organic Compounds in Cigarette Printing Varnish Based on Headspace-Gas Chromatography/Mass Spectrometry

建立了测定烟标印刷光油中挥发性有机物(苯及苯系物、溶剂残留、溶剂杂质)的顶空-气相色谱/质谱(HS-GC/MS)联用法。将光油试样经模拟打样方式印刷在白卡纸基,加入基质校正剂三乙酸甘油酯,在干燥温度80℃与干燥时间10 min的优化条件下,选择初温40℃,速率4℃/min升温至200℃的程序升温模式,采用氦气为恒定载气流,分流比20∶1的色谱参数,经Supelco Vocol专用挥发性有机化合物(VOCs)色谱柱分离,质量分析检测器定性分析,外标法定量分析。3类挥发性组分线性关系良好,相关系数(R^2)均高于0.9965;苯及苯系物、溶剂残留、溶剂杂质检出限(LOD,S/N=3)范围分别为0.001 mg/m^2、0.004~0.210 mg/m^2、0.001~0.180 mg/m^2;定量限(LOQ,S/N=10)范围分别为0.002~0.004 mg/m^2、0.012~0.680 mg/m^2、0.003~0.520 mg/m^2;不同浓度级别下的回收率高于85.2%,其相对标准偏差(RSD,n=5)小于6.2%。该方法分析快速准确,富集效率高,具有较高的灵敏度,适用于烟标印刷光油中溶剂残留的分析检测。

A headspace-gas chromatography/mass spectrometry(HS-GC/MS) method for volatile organic compounds(benzene series,solvent residues,solvent impurities) in the cigarette printing varnish was established.The varnish sample was printed on the white cardboard base by simulated proofing,and the matrix calibrator triacetin was added.Under the optimized conditions of 80 ℃ drying temperature and 10 min drying time,the programmed heating mode with initial temperature of 40 ℃ and rate of 4 ℃/min rising to 200 ℃ was selected.The chromatographic parameters with helium as a constant carrier gas and a split ratio of 20:1 were used for qualitative analysis.The samples were separated by a Supelco Vocol column and analyzed by a MSD detector with an external standard method for quantitative detection.The linear relationship of the three types of volatile components was good,and the correlation coefficients(R^2) were higher than 0.9965.The limits of detection of benzene series,solvent residues and solvent impurities(LODs,S/N=3) were 0.001 mg/m^2,0.004-0.210 mg/m^2 and 0.001-0.180 mg/m^2,respectively.The limits of quantification(LOQs,S/N=10) were 0.002-0.004 mg/m^2,0.012-0.680 mg/m^2 and 0.003-0.520 mg/m^2,respectively.The recovery rate at the concentration level was higher than 85.2%,and the relative standard deviation(RSD) was less than 6.2%(n=5).The method is rapid,accurate, and has high concentration efficiency and high sensitivity.It is suitable for the detection of solvent residue in cigarette label printing varnish.