Simultaneous determination of the residues of eight isocyanates in synthesized leathers using ultra performance liquid chromatography-orbitrap high resolution mass spectrometry

doi:10.3724/SP.J.1123.2016.04037

Abstract

Abstract:

An effective method of ultra performance liquid chromatography-orbitrap high resolution mass spectrometry (UPLC-Orbitrap HRMS) was established for the simultaneous determination of the residues of eight isocyanates in synthesized leathers. Residual isocyanates in synthesized leathers were ultrasonically extracted using dichloromethane as the extraction solvent and derivatized by 9-(methylaminomethyl) anthracene (MAMA) at the same time. The derivatives were concentrated and analyzed by UPLC-Orbitrap HRMS technique. The concentration of each analyte was calibrated by the external standard method. The derivatives were separated on a Hypersil GOLD column (100 mm×2.1 mm, 1.9 μm) with a gradient elution of acetonitrile and 0.1% (v/v) formic acid aqueous solution, and analyzed by Orbitrap HRMS in positive ESI mode. The qualitative analyses were carried out by the exact masses of quasi-molecular ions and the retention times. The quantitative analyses were carried out by the peak areas in extracted chromatograms. The limits of quantification (LOQs) were 0.2 μg/kg for all the eight isocyanates. The analytes were spiked in blank samples at three levels and the average recoveries varied from 85.41% to 95.53% with the relative standard deviations (RSDs) of 2.55%-6.87%. The proposed method was applied in the analysis of synthesized leather products and isophorone diisocyanate (IPDI) was detected in a real sample. The proposed method was accurate and sensitive, and applicable to the determination of the residues of isocyanates in synthesized leathers.

Key words: isocyanates, orbitrap high resolution mass spectrometry (Orbitrap HRMS), synthesized leathers, ultra performance liquid chromatography (UPLC)

CLC Number:

O658

WANG Chengyun, LI Lixia, LIN Junfeng, CHU Naiqing, XIE Tangtang. Simultaneous determination of the residues of eight isocyanates in synthesized leathers using ultra performance liquid chromatography-orbitrap high resolution mass spectrometry[J]. Chinese Journal of Chromatography, 2016, 34(9): 888-894.

References

[1] Yao H P, Guan J B. Polyurethane Industry, 2006, 21(5): 42 姚和平, 管军波. 聚氨酯工业, 2006, 21(5): 42
[2] Woolrich P F. Am Ind Hyg Assoc J, 1982, 43(2): 89
[3] Ji Y B, Jiang H, Lang L, et al. Journal of Toxicology, 2005, 19(3): 225 季宇斌, 蒋晖, 郎朗, 等. 毒理学杂志, 2005, 19(3): 225
[4] Zhou J P, Li J, Lin D F, et al. Journal of Environment and Health, 2008, 25(2): 120 周金鹏, 李杰, 林大枫, 等. 环境与健康杂志, 2008, 25(2): 120
[5] Zhang Y, Zhang X F, Wang W J, et al. Journal of Environment and Health, 2008, 25(5): 395 张旸, 张晓峰, 王蕴佳, 等. 环境与健康杂志, 2008, 25(5): 395
[6] Wu Z J, Zhou J P, Du J W. Journal of Environment and Health, 2009, 26(5): 417 吴子俊, 周金鹏, 杜建伟. 环境与健康杂志, 2009, 26(5): 417
[7] Wu M, Chen S X, Zhou J P. Occupation and Health, 2015, 31(5): 601 吴梅, 陈胜雄, 周金鹏. 职业与健康, 2015, 31(5): 601
[8] Cong J K, Zhao B, Yang F Z, et al. Journal of Hebei Normal University: Natural Science Edition, 2008, 32(1): 78 丛继坤, 赵博, 杨福祯, 等. 河北师范大学学报: 自然科学版, 2008, 32(1): 78
[9] Guo X D, Xian Y P, Du Z F, et al. Modern Food Science and Technology, 2008, 24(9): 937 郭新东, 冼燕萍, 杜志峰, 等. 现代食品科技, 2008, 24(9): 937
[10] Han W, Wang L B, Zhao Q, et al. Chinese Journal of Analytical Chemistry, 2010, 38(9): 1337 韩伟, 王利兵, 赵青, 等. 分析化学, 2010, 38(9): 1337
[11] Lai Y, Lin R, Huang Z P, et al. Physical Testing and Chemical Analysis Part B: Chemical Analysis, 2014, 50(10): 1223 赖莺, 林睿, 黄宗平, 等. 理化检验-化学分册, 2014, 50(10): 1223
[12] Chen J Q, Yang Y R. The Light & Textile Industries of Fujian, 2015(2): 41 陈金泉, 杨瑜榕. 福建轻纺, 2015(2): 41
[13] Gagne S, Lesage J, Ostiguy C, et al. J Environ Monit, 2005, 7: 145
[14] Li J Q, Zhou Y F, Ding J H, et al. Chinese Journal of Analytical Chemistry, 2008, 36(9): 1300 李建强, 周瑜芳, 丁健桦, 等. 分析化学, 2008, 36(9): 1300
[15] Chen M L, Fei D, Zhu Y. Chinese Journal of Analysis Laboratory, 2008, 27(7): 78 陈梅兰, 费栋, 朱岩. 分析试验室, 2008, 27(7): 78
[16] Xiang Z C, Xian D Q, Liu P C, et al. Journal of Environment and Health, 2011, 28(11): 1002 向仲朝, 先德强, 刘鹏程, 等. 环境与健康杂志, 2011, 28(11): 1002
[17] Xiong Z Q, Wang L B, Li N T, et al. Journal of Instrumental Analysis, 2012, 31(1): 104 熊中强, 王利兵, 李宁涛, 等. 分析测试学报, 2012, 31(1): 104
[18] Feng Z Z, Huang H H, Che L D, et al. Journal of Instrumental Analysis, 2012, 31(Suppl): 62 冯真真, 黄红花, 车礼东, 等. 分析测试学报, 2012, 31(增刊): 62
[19] Andre C, Jorge F, Castanheira I, et al. J Chemom, 2013, 27: 91
[20] Zhao T T, Xi S F, Li H Y, et al. Chinese Journal of Analysis Laboratory, 2014, 33(7): 835 赵田甜, 席绍峰, 李慧勇, 等. 分析试验室, 2014, 33(7): 835
[21] Seiwert B, Henneken H, Karst U. J Am Soc Mass Spectrom, 2004, 15: 1727
[22] Liu X L, Zeng X H, Huang C R, et al. Journal of Instrumental Analysis, 2008, 27(Suppl): 256 刘秀玲, 曾宪海, 黄长荣, 等. 分析测试学报, 2008, 27(增刊): 256
[23] Gagne S, Lesage J, Ostiguy C, et al. Analyst, 2003, 128: 1447
[24] Guo Q Z, Du Z X. Journal of Chinese Mass Spectrometry Society, 2011, 32(2): 112 郭巧珍, 杜振霞. 质谱学报, 2011, 32(2): 112
[25] Wang J C, Zhang H J, Chen J P. Journal of Instrumental Analysis, 2013, 32(9): 1056 王金成, 张海军, 陈吉平. 分析测试学报, 2013, 32(9): 1056
[26] Du Y S, Li Q, Wu C M, et al. Chinese Journal of Chromatography, 2015, 33(4): 371 杜彦山, 李强, 吴春敏, 等. 色谱, 2015, 33(4): 371
[27] Ye X W, Peng Y, Niu Z Y, et al. Chinese Journal of Chromatography, 2015, 33(4): 377 叶曦雯, 彭燕, 牛增元, 等. 色谱, 2015, 33(4): 377
[28] Zhao S Z, Yi X H, Shi Y Y, et al. Chinese Journal of Chromatography, 2016, 34(4): 397 赵善贞, 伊雄海, 时逸吟, 等. 色谱, 2016, 34(4): 397
[29] Zhang X G, Zheng Y J, Zeng Y T, et al. Chinese Journal of Chromatography, 2015, 33(6): 583 张协光, 郑彦婕, 曾泳艇, 等. 色谱, 2015, 33(6): 583
[30] Wang C Y, Zhu N Q, Lin J F, et al. Cotton Textiles Technology, 2016, 44(5): 71 王成云, 褚乃清, 林君峰, 等. 棉纺织技术, 2016, 44(5): 71