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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
引用本文:郭蕾蕾,李莹,李海山,连增斌.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[J].色谱,2018,36(12):1342-1348.
作者姓名:郭蕾蕾  李莹  李海山  连增斌
作者单位:1. 昆明理工大学, 云南 昆明 650504; 2. 昆明瑞丰印刷有限公司, 云南 昆明 650217
基金项目:昆明理工大学科技开发项目(KKK0201701083).
摘    要: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。

关 键 词:顶空-气相色谱-质谱联用法  溶剂残留  挥发性有机化合物  模拟印刷  紫外光固化胶印油墨
收稿时间:2018-09-05

Simultaneous determination of 27 solvent residuals in ultraviolet curable offset inks by headspace gas chromatography-mass spectrometry
GUO Leilei,LI Ying,LI Haishan,LIAN Zengbin.Simultaneous determination of 27 solvent residuals in ultraviolet curable offset inks by headspace gas chromatography-mass spectrometry[J].Chinese Journal of Chromatography,2018,36(12):1342-1348.
Authors:GUO Leilei  LI Ying  LI Haishan  LIAN Zengbin
Institution:1. Kunming University of Science and Technology, Kunming 650504, China; 2. Kunming Richfun Printing Co., Ltd., Kunming 650217, China
Abstract: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 (R2) no lower than 0.9950. The limits of detection (S/N=3) were in the range of 0.001-0.310 mg/m2 and the limits of quantification (S/N=10) were in the range of 0.003-0.920 mg/m2. 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.
Keywords:headspace gas chromatography-mass spectrometry (HS-GC-MS)  solvent residuals  volatile organic compounds (VOCs)  analog printing  ultraviolet curable offset inks
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