Determination and identification of acrylamide residues in poly-acrylamide by ultra-performance liquid chromatography-quadrupole electrostatic field orbitrap high-resolution mass spectrometry

doi:10.3724/SP.J.1123.2017.08014

Abstract

Abstract:

A new method for the direct determination of acrylamide residues in poly-acrylamide (PAM) by ultra-performance liquid chromatography (UPLC)-quadrupole electrostatic field orbitrap high-resolution mass spectrometry with the Hypercarb column was developed. With being diluted by water, the PAM sample was dissolved well by high-speed stirring. After filtering through a 0.22 μm aqueous phase microporous membrane, the sample was analyzed by high-resolution mass spectrometry directly. Chromatographic analysis was carried out using a Hypercarb column, distilled water and methanol applied as the mobile phases. In addition, the column temperature was strictly set at 20℃. The sample was determined in the mode of parallel reaction monitoring (PRM). Accurate mass-to-charge ratio extraction of the target compound ion and its fragment ion were utilized with elemental composition analysis and isotope distribution of the fragment ion to further improve the accuracy of qualitative and quantitative analysis. Meanwhile, the fragmentation pattern of acrylamide was acquired. The calibration curve showed a good linearity in the range of 2-50 μg/L with the correlation coefficient of 0.9998. The limit of detection (LOD) was 1.5 μg/kg, satisfying the detection demands. The recoveries of the acrylamide were in the range of 101.3%-107.1%. The relative standard deviations (RSD) were 3.1%-4.1%. The applications indicated that the mass percentages of AM in PAM were in the range of 0-0.43%. The proposed method is easy, fast, sensitive and suitable for the determination and confirmation of acrylamide residues in PAM.

Key words: acrylamide (AM), poly-acrylamide (PAM), quadrupole electrostatic field orbitrap high-resolution mass spectrometry, ultra-performance liquid chromatography (UPLC)

CLC Number:

O658

WANG Chenglong, ZHAO Jinli, LI Yanying, LIANG Lanlan, QI Ping. Determination and identification of acrylamide residues in poly-acrylamide by ultra-performance liquid chromatography-quadrupole electrostatic field orbitrap high-resolution mass spectrometry[J]. Chinese Journal of Chromatography, 2017, 35(12): 1294-1300.

References

1] Shao Z B, Zhou J S, Sun G, et al. Oilfield Chemistry, 2005, 22(1):72邵振波, 周吉生, 孙刚, 等. 油田化学, 2005, 22(1):72
[2] Yu R H. Petrochemical Industry Technology, 2016, 23(10):16余荣和. 石化技术, 2016, 23(10):16
[3] Chen F S, Liu Q Y. Papermaking Equipment & Materials, 2015(2):36陈夫山, 刘庆云. 造纸化学品及应用, 2015(2):36
[4] International Agency for Research on Cancer (IARC). Monographs on the Evaluation of Carcinogenic Risks to Humans. Lyon:International Agency for Research on Cancer, 2016
[5] Song Y, Li N. Journal of Hygiene Research, 2005, 34(2):241宋雁, 李宁. 卫生研究, 2005, 34(2):241
[6] GB 31629-2014
[7] Huang H X. Food & Machinery, 2010, 26(4):73黄红霞. 食品与机械, 2010, 26(4):73
[8] GB/T 31246-2014
[9] Gou S H, Cai X X, Ye Z B, et al. Applied Chemical Industry, 2014, 43(4):746苟绍华, 蔡潇潇, 叶仲斌, 等. 应用化工, 2014, 43(4):746
[10] Cai W H, Xian Y P, Luo H Y, et al. Modern Food Science and Technology, 2014, 30(2):249蔡玮红, 冼燕萍, 罗海英, 等. 现代食品科技, 2014, 30(2):249
[11] GB 5009.204-2014
[12] Fei Y L, Wang L R, Li S G. Science and Technology of Cereals, Oils and Foods, 2015, 23(1):70费永乐, 王丽然, 李书国, 等. 粮油食品科技, 2015, 23(1):70
[13] Yin Y B, Bian H W, Li B, et al. Food Science and Technology, 2017, 42(5):284阴永波, 卞华伟, 李冰, 等. 食品科技, 2017, 42(5):284
[14] Zhou Y F, Chen J, Du S S, et al. Modern Chemical Research, 2017(4):124周永芳, 陈际, 杜双双, 等. 当代化工研究, 2017(4):124
[15] Jiang J B, Chang Q, Luo Y, et al. Hebei Journal of Industrial Science and Technology, 2017, 34(1):71姜建彪, 常青, 罗毅, 等. 河北工业科技, 2017, 34(1):71
[16] Luo L, Ren Y, Liu J. Modern Preventive Medicine, 2016, 43(7):1187罗兰, 任燕, 柳洁, 等. 现代预防医学, 2016, 43(7):1187
[17] Hamid R N, Wan A W I, Muhammad A K, et al. Food Chem, 2018(239):208
[18] Wang J, Chow W, Leung D, et al. Food Chem, 2012, 60(49):12088
[19] Ganna F, Tomas R, Richard H L, et al. Mass Spectrum, 2013, 27(15):1751
[20] Huang X, Li S P, Zhang Y, et al. Chinese Journal of Analytical Chemistry, 2016, 44(11):1652黄鑫, 李帅坪, 张勇, 等. 分析化学, 2016, 44(11):1652
[21] Ross P.[PhD Dissertation]. Edinburgh:Edinburgh University, 1999
[22] 2002/657/EC
[23] Yen H Y, Yang M H. Polym Test, 2003(22):129
[24] Li S J, Jia J Y, Liu G Y, et al. J Chromatogr B, 2008, 870(1):63
[25] Wang Q. Science & Technology for Development, 2010(2):24王栖. 科学促进发展, 2010(2):24

[1]	DONG Yalei, NIU Shuijiao, QIAO Yasen, HUANG Chuanfeng, WANG Haiyan, SUN Lei. Determination of 19 illegally added chemical ingredients in hair loss prevention cosmetics by ultra-performance liquid chromatography-quadrupole-time of flight mass spectrometry [J]. Chinese Journal of Chromatography, 2022, 40(4): 343-353.
[2]	XIONG Yue, WANG Cheng, LIU Jianhui, SHI Huihui, WANG Yunhua, SUN Yao, YU Jie. Confirmation of unknown additives in enrofloxacin powder [J]. Chinese Journal of Chromatography, 2021, 39(6): 633-641.
[3]	QIAO Yongsheng, WANG Junhu, QIU Yajing, QIAN Zhongyi, HU Hui, CHEN Wei, WANG Ping. Establishment of screening and confirmation method for the analysis of pesticide residues in tea by ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry [J]. Chinese Journal of Chromatography, 2020, 38(12): 1402-1412.
[4]	WENG Zhongya, XUE Yun, SHI Wenjun, WANG Yan, YAN Chao. Preparation of a new organic-silica hybrid monolithic column and its applications in capillary liquid chromatography and pressurized capillary electrochromatography [J]. Chinese Journal of Chromatography, 2016, 34(5): 467-472.
[5]	ZHANG Cuiying, CHEN Shilin, DONG Liang. Analysis and assessment of four commercial products of Asian ginseng by ultra-performance liquid chromatography and chemometric analysis [J]. Chinese Journal of Chromatography, 2015, 33(5): 514-521.
[6]	YE Xiwen, PENG Yan, NIU Zengyuan, GAO Yonggang, LUO Xin, ZOU Li. Determination of free carcinogenic aromatic amines in textiles by ultra-performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry [J]. Chinese Journal of Chromatography, 2015, 33(4): 377-382.
[7]	XU Juan, WANG Lan, HUANG Huajun, CHEN Jie, CHEN Wenrui, XIANG Dapeng. Low temperature freezing followed by dispersive solid phase extraction for the determination of 104 pesticide residues in vegetable oils using ultra-performance liquid chromatography-tandem mass spectrometry [J]. Chinese Journal of Chromatography, 2015, 33(3): 242-249.
[8]	YE Xiwen, PENG Yan, NIU Zengyuan, GAO Yonggang, LUO Xin, ZOU Li, ZHOU Minghui. Identification of banned aromatic amines and their isomers in textiles by ultra-performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry [J]. Chinese Journal of Chromatography, 2014, 32(9): 1005-1012.
[9]	CHEN Limei1,2, SHANG Yanfen2, ZHAO Mengbin2, LIU Huwei1*. Rapid determination of 18 amino acids in soy sauce by ultra-performance liquid chromatography with pre-column derivatization [J]. Chinese Journal of Chromatography, 2010, 28(12): 1154-1157.
[10]	CHEN Lanzhen, LI Guifen, XUE Xiaofeng, WU Liming, ZHAO Jing, HUANG Jingping, YUAN Hancheng. Extraction and ultra-performance liquid chromatographic analysis of adenosine phosphates in royal jelly [J]. Chinese Journal of Chromatography, 2008, 26(6): 736-739.
[11]	LI Yi, ZHAO Jing, XUE Xiaofeng, ZHOU Jinhui. Determination of Twelve Active Compounds in Propolis Using Ultra-Performance Liquid Chromatography [J]. Chinese Journal of Chromatography, 2007, 25(6): 857-860.