顶空-气相色谱-质谱联用法同时测定紫外光固化胶印油墨中27种溶剂残留

Simultaneous determination of 27 solvent residuals in ultraviolet curable offset inks by headspace gas chromatography-mass spectrometry

建立了同时测定紫外光固化(UV)胶印油墨中27种溶剂残留(挥发性有机化合物,VOCs)的顶空-气相色谱-质谱联用(HS-GC-MS)法。将UV胶印油墨样品模拟印刷制成一定面积、厚度的试样,在紫外灯下烘烤1 min,经80℃、45 min静态顶空后,通过VOC专用毛细管柱分离和质谱检测,外标法定量。27种VOCs均呈现良好的线性关系,相关系数(R2)均≥0. 995 0;方法的检出限(LODs,S/N=3)为0. 001～0. 310 mg/m2,定量限(LOQs,S/N=10)为0. 003～0. 920 mg/m2;样品的平均加标回收率为80%～108%,相对标准偏差(RSD)<6%(n=6)。该方法制样便捷,灵敏度高,精密度好,准确度高,将其应用于实际UV胶印油墨样品的检测,取得了良好效果。

A headspace gas chromatography-mass spectrometry(HS-GC-MS)method was developed for the determination of 27 solvent residuals(volatile organic compounds,VOCs)in ultraviolet(UV)curable offset inks.Ink samples of a given area and thickness were prepared using an ink-scraping instrument and baked under a UV lamp for 1 min.The experimental conditions such as headspace temperature and time,and the GC-MS analytical conditions,were optimized.The ink samples were treated at 80℃for 45 min,and the evolved products were separated on a special VOC column,identified by MS,and quantified by an external-standard method.The calibration curves for all 27 VOCs showed good linearity with correlation coefficients(R 2)no lower than 0.995 0.The limits of detection(S/N=3)were in the range of 0.001-0.310 mg/m 2 and the limits of quantification(S/N=10)were in the range of 0.003-0.920 mg/m 2.The average recoveries of the 27 VOCs ranged from 80%to 108%at various spiked levels,with relative standard deviations less than 6%(n=6).Thus,this method has a high sensitivity and good precision and accuracy,and it is suitable for the determination of 27 solvent residuals in various UV offset inks.