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

doi:10.3724/SP.J.1123.2018.09010

色谱 ›› 2018, Vol. 36 ›› Issue (12): 1342-1348.DOI: 10.3724/SP.J.1123.2018.09010

• 技术与应用 • 上一篇

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

郭蕾蕾¹, 李莹¹, 李海山², 连增斌²

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

收稿日期:2018-09-05 出版日期:2018-12-08 发布日期:2014-11-06
通讯作者: 李莹,E-mail:haishanying@126.com
基金资助:
昆明理工大学科技开发项目（KKK0201701083）.

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

GUO Leilei¹, LI Ying¹, LI Haishan², LIAN Zengbin²

1. Kunming University of Science and Technology, Kunming 650504, China;
2. Kunming Richfun Printing Co., Ltd., Kunming 650217, China

Received:2018-09-05 Online:2018-12-08 Published:2014-11-06
Supported by:
Science and Technology Developing Project of Kunming University of Science and Technology (No. KKK0201701083).

摘要/Abstract

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≥0.9950；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, 挥发性有机化合物, 模拟印刷, 溶剂残留, 紫外光固化胶印油墨

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.

Key words: analog printing, headspace gas chromatography-mass spectrometry (HS-GC-MS), solvent residuals, ultraviolet curable offset inks, volatile organic compounds (VOCs)

中图分类号:

O658

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.

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.

参考文献

[1] Qi C. Printing Quality & Standardization, 2004(11):38 齐成. 印刷质量与标准化, 2004(11):38
[2] Wang X B.[MS Dissertation]. Wuxi:Jiangnan University, 2009 王晓兵.[硕士学位论文]. 无锡:江南大学, 2009
[3] Huang C X, Wang Z W, Wang S F. Packaging Engineering, 2007, 28(7):12 黄崇杏, 王志伟, 王双飞. 包装工程, 2007, 28(7):12
[4] Tang H, Jiang X L, Ren X M, et al. Fujian Analysis & Testing, 2017, 26(5):1 唐泓, 姜晓黎, 任晓梦, 等. 福建分析测试, 2017, 26(5):1
[5] Salmerón I, Loeza-Serrano S, Pérez-Vega S, et al. Food Sci Biotechnol, 2015, 24(2):1363
[6] Arnoldi S, Roda G, Coceanig A, et al. Forensic Toxicol, 2016, 34(2):411
[7] Yang J, Duan Y X, Zhao W, et al. Tobacco Science & Technology, 2015, 48(4):42 杨继, 段沅杏, 赵伟, 等. 烟草科技, 2015, 48(4):42
[8] Yang Y Q, Yuan K L, Chu G H, et al. Physical Testing and Chemical Analysis (Part B:Chem Anal), 2016, 52(8):894 杨艳芹, 袁凯龙, 储国海, 等. 理化检测(化学分册), 2016, 52(8):894
[9] Verissimo M I S, Gamelas J A F, Evtuguin D V, et al. Food Chem, 2017, 220:420
[10] Geng M, Tian F X, Xu B, et al. Environmental Protection Science, 2013, 39(4):7 耿明, 田富箱, 徐斌, 等. 环境保护科学, 2013, 39(4):7
[11] Salemi A, Lacorte S, Bagheri H, et al. J Chromatogr A, 2006, 1136(2):170
[12] Ma H L, Jin J, Li Y, et al. Chinese Journal of Chromatography, 2017, 35(10):1094 马慧莲, 金静, 李云, 等. 色谱, 2017, 35(10):1094
[13] Zhou Y M, Jiang K. Environmental Science Survey, 2018, 37(4):81 周勇明, 蒋凯. 环境科学导刊, 2018, 37(4):81
[14] Mucédola V, Vieira L, Pierone D, et al. Talanta, 2017, 164:470
[15] Li Y L, Wei J H, Sun W, et al. Packaging Engineering, 2012, 33(11):57 李亚玲, 魏建华, 孙雯, 等. 包装工程, 2012, 33(11):57
[16] Yang Y, Hou Y, Yang L, et al. Yunnan Chemical Technology, 2007(6):28 杨勇, 侯英, 杨蕾, 等. 云南化工, 2007(6):28
[17] Cao H Y, Jiang C Q, Yang S, et al. Chinese Agricultural Science Bulletin, 2015, 31(18):214 曹红云, 蒋次清, 杨帅, 等. 中国农学通报, 2015, 31(18):214
[18] Li Z H, Li X, Wang Q H, et al. Modern Food Science and Technology, 2011, 27(5):587 李中皓, 李雪, 王庆华, 等. 现代食品科技, 2011, 27(5):587
[19] Shi L Y, Zhao N, Chen R, et al. China Standardization, 2018(12):187 时丽艳, 赵娜, 陈锐, 等. 中国标准化, 2018(12):187
[20] Shi L L, Sun X, Chen Z T, et al. Journal of Inspection and Quarantine, 2018, 28(1):1 石玲玲, 孙欣, 陈章庭, 等. 检验检疫学刊, 2018, 28(1):1
[21] Zhao L, Feng W K, Mo S F, et al. Physical Testing and Chemical Analysis, 2017, 53(12):1375 赵历, 冯伟科, 莫少芳, 等. 理化检测, 2017, 53(12):1375
[22] Da J, Huang X L, Wang G L, et al. Chinese Journal of Chromatography, 2014, 32(11):1251 达晶, 黄湘鹭, 王钢力, 等. 色谱, 2014, 32(11):1251
[23] Lü Q, Zhang Q, Kang S Y, et al. Chinese Journal of Chromatography, 2010, 28(8):800 吕庆, 张庆, 康苏媛, 等. 色谱, 2010, 28(8):800
[24] Beaulieu J C, Stein-Chisholm R E. Food Chem, 2016, 190:643
[25] Hao H X, Zhou H, Liu X P, et al. Forensic Sci Int, 2013, 229(1/3):116
[26] Nie S P, Huang J G, Zhang Y N, et al. Food Control, 2013, 30(1):62

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

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