Citation: CHEN Ting, WEN Yuyun, OU Yan, GONG Zhenbin. Determination of N-nitrosamines in rubber products by solid phase extraction purification and ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(1): 89-94. doi: 10.3724/SP.J.1123.2013.08003 shu

Determination of N-nitrosamines in rubber products by solid phase extraction purification and ultra high performance liquid chromatography-tandem mass spectrometry

CHEN Ting ^1,3 ,
WEN Yuyun ^2,3 ,
OU Yan ² ,
GONG Zhenbin ^1,3,,

1.
1. State Key Laboratory of Marine Environmental Science, Xiamen University, Xiamen 361102, China;

Corresponding author: GONG Zhenbin,
Received Date: 1 August 2013
Available Online: 2 September 2013
Fund Project: 泉州市科技项目(2012FZ17). (2012FZ17)

A method using C₁₈ solid phase extraction (SPE) for purification and ultra high performance liquid chromatography (UHPLC) coupled with electrospray ionization tandem mass spectrometry (ESI-MS/MS) for detection was developed to simultaneously determine 13 N-nitrosamines in rubber products. The analytes were extracted with methanol (60 ℃, 30 min) with the aid of ultrasonic technique and then purified by a C₁₈ SPE cartridge. The analytes were separated on a C₁₈ chromatographic column and qualitatively and quantitatively detected by a mass spectrometer with positive ESI at multiple reaction monitoring (MRM) mode. The operating parameters for UHPLC separation and ESI-MS/MS detection were also optimized. Under optimum operating conditions, the relative standard deviations (RSDs, n=7) were less than 10% at spiked level of 50 μg/kg for all analytes except N-nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA) which were spiked at 500 μg/kg. The recoveries spiked in real samples were from 70.7% to 117.0%. The limits of detection (LODs, 10 times of standard deviation) were in the range of 0.5-500 μg/kg. The method has been successfully applied to the simultaneous determination of the 13 N-nitrosamines in rubber products.
1. [1]
  [1] Knight N, Watson K, Farre M J, et al. Environ Monit Assess, 2012, 184(7): 4207
2. [2]
  [2] Straif K, Weiland S K, Bungers M, et al. Occup Environ Med, 2000, 57(3): 180
3. [3]
  [3] Oury B, Limasset J C, Protois J C. Int Arch Occup Environ Health, 1997, 70(4): 261
4. [4]
  [4] EN 12868: 1999
5. [5]
  [5] 2009/48/EC
6. [6]
  [6] GB/T 24153-2009
7. [7]
  [7] Shen B, Zhu J H, Xu Q H. Chinese Journal of Analytical Chemistry (沈彬, 朱建华, 须沁华. 分析化学), 1998, 26(12): 1478
8. [8]
  [8] Wei F S, Xu X L, Zhou G H. Chinese Journal of Food Science (魏法山, 徐幸莲, 周光宏. 食品科学), 2008, 29(7): 479
9. [9]
  [9] Tao Y F, Huang H L, Zhang T Z. Chinese Journal of Instrumental Analysis (陶燕飞, 黄红林, 张桃芝. 分析测试学报), 2003, 22(5): 82
10. [10]
  [10] Ma Q, Xi H W, Wang C, et al. Chinese Journal of Analytical Chemistry (马强, 席海为, 王超, 等. 分析化学), 2011, 39(8): 1201
11. [11]
  [11] Xing Y N, Ni H G, Wang X, et al. Chinese Journal of Analytical Chemistry (幸苑娜, 倪宏刚, 王欣, 等. 分析化学), 2011, 39(7): 1065
12. [12]
  [12] Charrois J W A, Arend M W, Froese K L, et al. Environ Sci Technol, 2004, 38(18): 4835
13. [13]
  [13] Zhao Y Y, Boyd J, Hrudey S E, et al. Environ Sci Technol, 2006, 40(24): 7636
14. [14]
  [14] Wan W Y, Zhou W H, Zhang Y C, et al. Chinese Journal of Analysis Laboratory (万文亚, 周宛虹, 张怡春, 等. 分析试验室), 2012, 31(4): 69
15. [15]
  [15] Wang W F, Hu J Y, Yu J W, et al. Environ Sci Technol, 2010, 22(10): 1508
16. [16]
  [16] Sung J H, Kwak I S, Park S K, et al. Food Addit Contam, 2010, 27(12): 1745
17. [17]
  [17] Luo Q, Wang D H, Wang B Y, et al. Scientia Sinica Chimica (罗茜, 王东红, 王炳一, 等. 中国科学: 化学), 2011, 41(1): 82
18. [18]
  [18] Zhu W J, Yang J, Liu B Z, et al. Chinese Journal of Instrumental Analysis (朱文静, 杨俊, 刘百战, 等. 分析测试学报), 2010, 29(1): 26
19. [19]
  [19] Zhao H, Wang X Y, Wang P Y, et al. Chinese Journal of Chromatography (赵华, 王秀元, 王萍亚, 等. 色谱), 2013, 31(3): 223
20. [20]
  [20] Xian Q M, Huang P L. Chinese Journal of Instrumental Analysis (鲜启明, 黄沛力. 分析测试学报), 2008, 27(4): 445
21. [21]
  [21] Yang R J, Dai X W, Wei B W, et al. Chinese Journal of Environmental Chemistry (杨荣静, 戴雪伟, 卫碧文, 等. 环境化学), 2012, 31(8): 1283
22. [22]
  [22] Liu Q M, Zhang X C, Zhou Q, et al. Chinese Journal of Environmental Chemistry (刘清明, 张雪晨, 周全, 等. 环境化学), 2011, 30(7): 1327
23. [23]
  [23] Incavo J A, Schafer M A. Anal Chim Acta, 2006, 557(15): 256
1. [1]
  Yanhui Zhong , Ran Wang , Zian Lin . Analysis of Halogenated Quinone Compounds in Environmental Water by Dispersive Solid-Phase Extraction with Liquid Chromatography-Triple Quadrupole Mass Spectrometry. University Chemistry, 2024, 39(11): 296-303. doi: 10.12461/PKU.DXHX202402017
2. [2]
  Zunxiang Zeng , Yuling Hu , Yufei Hu , Hua Xiao . Analysis of Plant Essential Oils by Supercritical CO₂Extraction with Gas Chromatography-Mass Spectrometry: An Instrumental Analysis Comprehensive Experiment Teaching Reform. University Chemistry, 2024, 39(3): 274-282. doi: 10.3866/PKU.DXHX202309069
3. [3]
  Yifan Xie , Liyun Yao , Ruolin Yang , Yuxing Cai , Yujie Jin , Ning Li . Exploration and Practice of Online and Offline Hybrid Teaching Mode in High-Performance Liquid Chromatography Experiment. University Chemistry, 2025, 40(11): 100-107. doi: 10.12461/PKU.DXHX202412133
4. [4]
  Chongjing Liu , Yujian Xia , Pengjun Zhang , Shiqiang Wei , Dengfeng Cao , Beibei Sheng , Yongheng Chu , Shuangming Chen , Li Song , Xiaosong Liu . Understanding Solid-Gas and Solid-Liquid Interfaces through Near Ambient Pressure X-Ray Photoelectron Spectroscopy. Acta Physico-Chimica Sinica, 2025, 41(2): 100013-0. doi: 10.3866/PKU.WHXB202309036
5. [5]
  Mingyang Men , Jinghua Wu , Gaozhan Liu , Jing Zhang , Nini Zhang , Xiayin Yao . Sulfide Solid Electrolyte Synthesized by Liquid Phase Approach and Application in All-Solid-State Lithium Batteries. Acta Physico-Chimica Sinica, 2025, 41(1): 100004-0. doi: 10.3866/PKU.WHXB202309019
6. [6]
  Runjie Li , Hang Liu , Xisheng Wang , Wanqun Zhang , Wanqun Hu , Kaiping Yang , Qiang Zhou , Si Liu , Pingping Zhu , Wei Shao . 氨基酸的衍生及手性气相色谱分离创新实验. University Chemistry, 2025, 40(6): 286-295. doi: 10.12461/PKU.DXHX202407059
7. [7]
  Gaoyan Chen , Chaoyue Wang , Juanjuan Gao , Junke Wang , Yingxiao Zong , Kin Shing Chan . Heart to Heart: Exploring Cardiac CT. University Chemistry, 2024, 39(9): 146-150. doi: 10.12461/PKU.DXHX202402011
8. [8]
  Ke Qiu , Fengmei Wang , Mochou Liao , Kerun Zhu , Jiawei Chen , Wei Zhang , Yongyao Xia , Xiaoli Dong , Fei Wang . A Fumed SiO₂-based Composite Hydrogel Polymer Electrolyte for Near-Neutral Zinc-Air Batteries. Acta Physico-Chimica Sinica, 2024, 40(3): 2304036-0. doi: 10.3866/PKU.WHXB202304036
9. [9]
  Caixia Lin , Ting Liu , Zhaojiang Shi , Hong Yan , Keyin Ye , Yaofeng Yuan . Innovative Experiment of Electrochemical Dearomative Spirocyclization of N-Acyl Sulfonamides. University Chemistry, 2025, 40(4): 359-366. doi: 10.12461/PKU.DXHX202406107
10. [10]
  Cong-Bin Ji , Ding-Xiong Xie , Mei Chen , Ye-Ying Lan , Bao-Hua Zhang , Ji-Ying Yang , Zheng-Hui Kang , Shu-Jie Chen , Yu-Wei Zhang , Yun-Lin Liu . Green synthesis of 2-trifluoromethylquinoline skeletons via organocatalytic N-[(α-trifluoromethyl)vinyl]isatins CN bond activation. Chinese Chemical Letters, 2025, 36(7): 110598-. doi: 10.1016/j.cclet.2024.110598
11. [11]
  Shunü Peng , Huamin Li , Zhaobin Chen , Yiru Wang . Simultaneous Application of Multiple Quantitative Analysis Methods in Gas Chromatography for the Determination of Active Ingredients in Traditional Chinese Medicine Preparations. University Chemistry, 2025, 40(10): 243-249. doi: 10.12461/PKU.DXHX202412043
12. [12]
  Chunai Dai , Yongsheng Han , Luting Yan , Zhen Li , Yingze Cao . Ideological and Political Design of Solid-liquid Contact Angle Measurement Experiment. University Chemistry, 2024, 39(2): 28-33. doi: 10.3866/PKU.DXHX202306065
13. [13]
  Xiaowu Zhang , Pai Liu , Qishen Huang , Shufeng Pang , Zhiming Gao , Yunhong Zhang . Acid-Base Dissociation Equilibrium in Multiphase System: Effect of Gas. University Chemistry, 2024, 39(4): 387-394. doi: 10.3866/PKU.DXHX202310021
14. [14]
  Yajie Li , Bin Chen , Yiping Wang , Hui Xing , Wei Zhao , Geng Zhang , Siqi Shi . Inhibiting Dendrite Growth by Customizing Electrolyte or Separator to Achieve Anisotropic Lithium-Ion Transport: A Phase-Field Study. Acta Physico-Chimica Sinica, 2024, 40(3): 2305053-0. doi: 10.3866/PKU.WHXB202305053
15. [15]
  Xiaofeng Xia , Jielian Zhu . Innovative Comprehensive Experimental Design: Synthesis of 6-Fluoro-N-benzoyl Tetrahydroquinoline. University Chemistry, 2024, 39(10): 344-352. doi: 10.12461/PKU.DXHX202405063
16. [16]
  Binbin Liu , Yang Chen , Tianci Jia , Chen Chen , Zhanghao Wu , Yuhui Liu , Yuhang Zhai , Tianshu Ma , Changlei Wang . Hydroxyl-functionalized molecular engineering mitigates 2D phase barriers for efficient wide-bandgap and all-perovskite tandem solar cells. Acta Physico-Chimica Sinica, 2026, 42(1): 100128-0. doi: 10.1016/j.actphy.2025.100128
17. [17]
  Jiayao Wang , Guixu Pan , Ning Wang , Shihan Wang , Yaolin Zhu , Yunfeng Li . Preparation of donor-π-acceptor type graphitic carbon nitride photocatalytic systems via molecular level regulation for high-efficient H₂O₂ production. Acta Physico-Chimica Sinica, 2025, 41(12): 100168-0. doi: 10.1016/j.actphy.2025.100168
18. [18]
  Lirui Shen , Kun Liu , Ying Yang , Dongwan Li , Wengui Chang . Synthesis and Application of Decanedioic Acid-N-Hydroxysuccinimide Ester: Exploration of Teaching Reform in Comprehensive Applied Chemistry Experiment. University Chemistry, 2024, 39(8): 212-220. doi: 10.3866/PKU.DXHX202312035
19. [19]
  Junjun Huang , Ran Chen , Yajian Huang , Hang Zhang , Anran Zheng , Qing Xiao , Dan Wu , Ruxia Duan , Zhi Zhou , Fei He , Wei Yi . Discovery of an enantiopure N-[2-hydroxy-3-phenyl piperazine propyl]-aromatic carboxamide derivative as highly selective α_1D/1A-adrenoceptor antagonist and homology modelling. Chinese Chemical Letters, 2024, 35(11): 109594-. doi: 10.1016/j.cclet.2024.109594
20. [20]
  Huixian Weng , Lefei Hu , Lei Hu , Yihan Zhou , Aohua Wang , Ning Wang , Wenzhe Li , Chunliu Zhu , Shiyan Guo , Miaorong Yu , Yong Gan . Corrigendum to "The complexation of insulin with sodium N-[8-(2-hydroxybenzoyl)amino]-caprylate for enhanced oral delivery: Effects of concentration, ratio, and pH" [Chinese Chemical Letters 33 (2022) 1889-1894]. Chinese Chemical Letters, 2025, 36(8): 111316-. doi: 10.1016/j.cclet.2025.111316

Get Citation

PDF

XML

Metrics

PDF Downloads(0)
Abstract views(529)
HTML views(25)

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