超高效液相色谱-三重四极杆质谱法检测油脂和油炸食品中7种杂环胺类物质

引用本文: 张晨霞, 马宇翔, 赵天培, 席俊, 李潘, 郭庆, 史莉莉, 汪学德. 超高效液相色谱-三重四极杆质谱法检测油脂和油炸食品中7种杂环胺类物质[J]. 色谱, 2020, 38(2): 224-231. doi: 10.3724/SP.J.1123.2019.04046 shu

Citation: ZHANG Chenxia, MA Yuxiang, ZHAO Tianpei, XI Jun, LI Pan, GUO Qing, SHI Lili, WANG Xuede. Determination of seven heterocyclic aromatic amines in oils and fried foods by ultra performance liquid chromatography-triple quadrupole mass spectrometry[J]. Chinese Journal of Chromatography, 2020, 38(2): 224-231. doi: 10.3724/SP.J.1123.2019.04046 shu

超高效液相色谱-三重四极杆质谱法检测油脂和油炸食品中7种杂环胺类物质

河南工业大学粮油食品学院, 河南郑州 450001
基金项目:
国家重点研发计划（2017YFC1600402-3）；现代农业产业技术体系建设项目（CARS14-1-29）；河南工业大学"科教融合"项目（26400109）.

摘要: 建立了检测油脂及油炸食品中7种杂环胺类物质的超高效液相色谱-三重四极杆质谱（UPLC-MS/MS）的检测方法。以含1%（体积分数）氨水的乙腈溶液为提取液，采用乙腈饱和的正己烷脱脂，以PCX固相萃取柱为净化柱，10 mmol/L甲酸铵溶液（pH 6.8）和乙腈为流动相，采用Waters ACQUITY UPLC BEH C18反相色谱柱（50 mm×2.1 mm，1.7 μm）梯度洗脱，流速为0.3 mL/min，在正离子扫描、多反应监测模式下测定，内标法定量。结果表明，杂环胺类物质在各自范围内，线性关系良好，相关系数大于0.999；在3个加标水平下，杂环胺类物质在油脂和油炸食品中的平均回收率为64.31%~113.8%，相对标准偏差为0.18%~9.26%，检出限（S/N=3）和定量限（S/N=10）分别为0.01~0.14 ng/g和0.09~0.38 ng/g。该方法具有灵敏、准确等优点，适用于油脂和油炸食品中杂环胺的确证检测。

关键词:

English

Determination of seven heterocyclic aromatic amines in oils and fried foods by ultra performance liquid chromatography-triple quadrupole mass spectrometry

College of Food Science and Technology, Henan University of Technology, Zhengzhou 450001, China
Received Date: 29 April 2019
Fund Project:
National Key Research and Development Program of China (No. 2017YFC1600402-3)

Abstract: An ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS) method was developed for the determination of seven heterocyclic aromatic amines (HCAs) in oil and fried food samples. The samples were extracted with acetonitrile containing 1% (v/v) ammonia water, defatted by n-hexane saturated with acetonitrile, and cleaned up with PCX solid phase extraction column. The extracts were separated on a Waters ACQUITY UPLC BEH C18 reversed-phase column (50 mm×2.1 mm, 1.7 μm) with gradient elution by using acetonitrile-10 mmol/L ammonium formate aqueous solution as the mobile phase. Quantitative detection was performed by using a positive-ion electrospray ionization source in the multiple reaction monitoring (MRM) mode, employing an internal isotope standard. The method showed good linear relationships in the range of 0.5-100 μg/L for the seven HCAs with correlation coefficients (R²)>0.999. The average recoveries ranged from 64.31% to 113.8% with the relative standard deviations of 0.18%-9.26% at the three spiked levels in oil and fried food samples. The limits of detection (LODs) and limits of quantification (LOQs) were 0.01-0.14 ng/g and 0.09-0.38 ng/g, respectively. The method is sensitive, accurate, and suitable for the determination and confirmation of the seven HCAs in oil and fried food samples.

Key words:

ultra performance liquid chromatography (UPLC)
/ triple quadrupole mass spectrometry (MS/MS)
/ solid phase extraction (SPE)
/ heterocyclic aromatic amines (HCAs)
/ oils
/ fried foods

1. [1] Li Y, He Z Y, Gao D M, et al. Journal of Food Safety and Quality, 2019, 10(2):312 李永, 何志勇, 高大明, 等. 食品安全质量检测学报, 2019, 10(2):312
2. [2] Sugimura T. Mutat Res-Fund Mol M, 1985, 150(1):33
3. [3] Bellamri M, Turesky R J. Encyclo of Food Chem, 2019:550
4. [4] Delannee V, Langouet S, Siegel A, et al. Toxicol Lett, 2019, 300:18
5. [5] Xie Y Y, Wang X X, Yan W J, et al. Food Research and Development, 2017, 38(15):199 谢洋洋, 王小溪, 闫文杰, 等. 食品研究与开发, 2017, 38(15):199
6. [6] Xiao S, Guo J, Yun B H, et al. Anal Chem, 2016, 88(24):12508
7. [7] Turesky R J, Paul V. J Chromatogr B, 2004, 802(1):155
8. [8] Niwa T, Yamazoe Y, Kato R. Mutat Res, 1982, 95(2/3):159
9. [9] Ito N, Hasegawa R, Sano M, et al. Carcinogenesis, 1991, 12(8):1503
10. [10] Jian S H, Yeh P J, Wang C H, et al. J Food Drug Anal, 2019, 27(2):595
11. [11] Barzegar F, Kamankesh M, Mohammadi A. Food Chem, 2019, 280:240
12. [12] Kato T, Ohgaki H, Hasegawa H, et al. Carcinogenesis, 1988, 9(1):71
13. [13] Wong D, Cheng K W, Wang M. Food Chem, 2012, 133(3):760
14. [14] Gross G A, Grüter A. J Chromatogr A, 1992, 592(1/2):271
15. [15] Skog K. Food Chem Toxicol, 2002, 40(8):1197
16. [16] Gibis M. Compr Rev Food Sci F, 2016, 15(2):269
17. [17] Wolk A. J Intern Med, 2017, 281(2):106
18. [18] Wang Y, Hui T, Zhang Y W, et al. Food Chem, 2015, 167:251
19. [19] Fei L, Kuhnle G K, Cheng Q. Food Control, 2018, 92:399
20. [20] Zamora R, Hidalgo F J. Rsc Adv, 2015, 5(13):9709
21. [21] Solyakov A, Skog K. Food Chem Toxicol, 2002, 40(8):1205
22. [22] Johansson M, Skog K, J Gerstad M. Carcinogenesis, 1993, 14(1):89
23. [23] Jinap S, Mohd Mokhtar M S, Farhadian A, et al. Meat Sci, 2013, 94(2):202
24. [24] Zamora R, Alcón E, Hidalgo F J. Food Chem, 2012, 135(4):2569
25. [25] Shao B, Peng Z Q, Yang H S, et al. Chinese Journal of Chromatography, 2011, 29(8):755 邵斌, 彭增起, 杨洪生, 等. 色谱, 2011, 29(8):755
26. [26] Turesky R J, Jason T, Laura S, et al. J Agric Food Chem, 2005, 53(8):3248
27. [27] Guo H T, Pan H, Wang Z Y, et al. Chinese Journal of Chromatography, 2012, 30(10):1074 郭海涛, 潘晗, 王振宇, 等. 色谱, 2012, 30(10):1074
28. [28] Xian Y P, Wu Y L, Dong H, et al. Food Chem, 2019, 285:77
29. [29] Zhang W F, Lan C, Zhang H M. J Agric Food Chem, 2019, 67(13):3733
30. [30] Barceló-Barrachina E, Moyano E, Galceran M T, et al. J Chromatogr A, 2006, 1125(2):195
31. [31] Zhang Y, Lin C, Fang G, et al. Eur Food Res Technol, 2012, 234(2):197
32. [32] Zhang Q C, Xiao X H, Li G K. Chinese Journal of Chromatography, 2014, 32(9):975 张仟春, 肖小华, 李攻科. 色谱, 2014, 32(9):975
33. [33] Yan Y, Zeng M, Zheng Z, et al. Anal Methods, 2014, 6(16):6437
34. [34] Yan Y, Zhang S, Tao G J, et al. J Chromatogr B, 2017, 1068:173
35. [35] Shi L K, Liu Y L. Journal of the Chinese Cereals and Oils Association, 2015, 30(12):114 石龙凯, 刘玉兰. 中国粮油学报, 2015, 30(12):114
36. [36] Liu Z C, Yang F, Yu K J, et al. Chinese Journal of Chromatography, 2012, 30(12):1253 刘正才, 杨方, 余孔捷, 等. 色谱, 2012, 30(12):1253
37. [37] Matuszewski B K, Constanzer M L, Chavez-Eng C M. Anal Chem, 1998, 70(5):882

扫一扫看文章

计量

PDF下载量: 6
文章访问数: 39
HTML全文浏览量: 2

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

超高效液相色谱-三重四极杆质谱法检测油脂和油炸食品中7种杂环胺类物质

English

Determination of seven heterocyclic aromatic amines in oils and fried foods by ultra performance liquid chromatography-triple quadrupole mass spectrometry

计量

文章相关

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处