Citation: YANG Hua-Mei, HANG Li, YANG Jian-Guo, ZHANG Xue-Mei, HUANG Wei-Hong, LI Chen, JIANG Xiao-Li. Ultra Liquid Chromatography-Tandem Mass Spectrometry with Dansyl Chloride Pre-column Derivatization[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(3): 462-467. doi: 10.11895/j.issn.0253-3820.150764 shu

Ultra Liquid Chromatography-Tandem Mass Spectrometry with Dansyl Chloride Pre-column Derivatization

1.
Taizhou Center for Disease Control and Prevention, Taizhou 225300, China

Corresponding author: YANG Hua-Mei,
Received Date: 28 September 2015
Available Online: 7 December 2015

A method was developed for the quantification of cyclohexylamine in human urine samples by ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) with pre-column derivatization. After the refrigerated centrifugation of urine samples, cyclohexylamine in supernatant was derived with dansyl chloride and then its derivant was purified with solid phase extraction (SPE). The target compounds were separated on a Waters ACQUITY CSHTM C₁₈ column (50 mm×2.1 mm, 1.7 μm) with the gradient elution of methanol and water (containing 0.002 mol/L ammonium acetate) and were determined in electrospray positive ionization (ESI⁺) and multiple reaction monitoring (MRM) modes. The linear range was 2.5-200 μg/L for cyclohexylamine with the correlation coefficient more than 0.999. The recovery ranged from 98.7% to 102.3%, with the relative standard deviations (RSDs) of 3.1%-5.2%. The limit of detection (LOD) and the limit of quantitation (LOQ) were 1 μg/L and 3 μg/L. The results indicated that the method was accurate and reliable, and suitable for the detection of cyclohexylamine in urine samples. The urine samples of 200 primary school students were analyzed by this method and the positive rate of cyclohexylamine was 34.5%.
- Cyclohexylamine,
- Dansyl chloride,
- Derivatization,
- Solid phase extraction,
- Human urine samples,
- Ultra liquid chromatography-tandem mass spectrometry
1. [1]
  1 YU Guo-Xin. China Food Safety, 2011, 10: 48-49余国新. 食品安全导刊, 2011, 10: 48-49
2. [2]
  2 HAN Hua, JI Yuan-Bing, LI Jie-Li, YOU Ji-Ming, LI Hong-Mei, YANG Kang-Zhen. Green Science and Technology, 2013, 3: 148-150韩华, 纪元兵, 李洁莉, 尤继明, 李红梅, 杨抗震. 绿色科技, 2013, (3): 48-150
3. [3]
  3 Price J M, Biava C G, Oser B L, Vogin E E, Steinfeld J, Ley H L. Science., 1970, 167: 1131-1132
4. [4]
  4 Mohd I, Deepak M, Shaik N R, Sudhir K S, Tulsidas R B. J. Pharm. Bioallied. Sci., 2013, 5(1): 44-48
5. [5]
  5 Buss N E, Renwick A G, Donaldson K M, George C F. Toxicol. Appl. Pharmacol., 1992, 115: 199-210
6. [6]
  6 Takayama S, Renwick A G, Johansson S L, Thorgeirsson U P, Tsutsumi M, Dalgard D W, Sieber S M. Toxicol. Sci., 2000, 53: 33-39
7. [7]
  7 Serra-Majem L, Bassas L, García-Glosas R, Ribas L, Inglés C, Casals I, Saavedra P, Renwick A G. Food Addit Contam., 2003, 20: 1097-1104
8. [8]
  8 Andreatta M M, Muñoz S E, Lantieri M J, Eynard A R, Navarro A. Prev. Med., 2008, 47: 136-139
9. [9]
  9 Renwick A G, Thompson J P, O'Shaughnessy M, Walteret E J. Toxicol. Appl. Pharmacol., 2004, 196: 367-380
10. [10]
  10 Drassr B S, Renwick A G, Williams R T. J. Biochem., 1972, 129: 881-890
11. [11]
  11 LING Guan-Ting. Cereals & Oils., 2009, 3: 41-43凌关庭. 粮食与油脂, 2009, 3: 41-43
12. [12]
  12 YANG Qing. China Quality Supervision., 2010, 5: 35-37杨晴. 中国质量技术监督, 2010, 5: 35-37
13. [13]
  13 Prosky L, Dell R G. J. Pharm. Sci., 1971, 60: 1341-1343
14. [14]
  14 Renwick A G, Williams R T. J. Biochem., 1972, 129: 857-867
15. [15]
  15 Matsumura R, Kohei H. J. Chromatogr. A, 1976, 117: 383-391
16. [16]
  16 Isidre C, Maria R, Judith A, Margarita F, Lluis S M. J. Chromatogr. A, 1996, 750: 397-402
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]
  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
3. [3]
  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
4. [4]
  Yikai Wang , Xiaolin Jiang , Haoming Song , Nan Wei , Yifan Wang , Xinjun Xu , Cuihong Li , Hao Lu , Yahui Liu , Zhishan Bo . Thickness-Insensitive, Cyano-Modified Perylene Diimide Derivative as a Cathode Interlayer Material for High-Efficiency Organic Solar Cells. Acta Physico-Chimica Sinica, 2025, 41(3): 2406007-0. doi: 10.3866/PKU.WHXB202406007
5. [5]
  Jingjie Tang , Luying Xie , Jiayu Liu , Shangyu Shi , Xinyu Sun , Jiayang Lin , Qikun Yang , Chuan'ang Yu , Zecheng Wang , Yingying Wang , Zengyang Xie . Efficient Rapid Synthesis and Antibacterial Activities of Tosylhydrazones: A Recommended Innovative Chemistry Experiment for Undergraduate Medical University. University Chemistry, 2024, 39(3): 316-326. doi: 10.3866/PKU.DXHX202309091
6. [6]
  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
7. [7]
  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): 2309036-0. doi: 10.3866/PKU.WHXB202309036
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]
  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
10. [10]
  Bizhu Shao , Huijun Dong , Yunnan Gong , Jianhua Mei , Fengshi Cai , Jinbiao Liu , Dichang Zhong , Tongbu Lu . Metal-Organic Framework-Derived Nickel Nanoparticles for Efficient CO₂ Electroreduction in Wide Potential Windows. Acta Physico-Chimica Sinica, 2024, 40(4): 2305026-0. doi: 10.3866/PKU.WHXB202305026
11. [11]
  Xinlong XU , Chunxue JING , Yuzhen CHEN . Bimetallic MOF-74 and derivatives: Fabrication and efficient electrocatalytic biomass conversion. Chinese Journal of Inorganic Chemistry, 2025, 41(8): 1545-1554. doi: 10.11862/CJIC.20250046
12. [12]
  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
13. [13]
  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
14. [14]
  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
15. [15]
  Yongpo Zhang , Xinfeng Li , Yafei Song , Mengyao Sun , Congcong Yin , Chunyan Gao , Jinzhong Zhao . Synthesis of Chlorine-Bridged Binuclear Cu(I) Complexes Based on Conjugation-Driven Cu(II) Oxidized Secondary Amines. University Chemistry, 2024, 39(5): 44-51. doi: 10.3866/PKU.DXHX202309092
16. [16]
  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
17. [17]
  Jiao CHEN , Yi LI , Yi XIE , Dandan DIAO , Qiang XIAO . Vapor-phase transport of MFI nanosheets for the fabrication of ultrathin b-axis oriented zeolite membranes. Chinese Journal of Inorganic Chemistry, 2024, 40(3): 507-514. doi: 10.11862/CJIC.20230403
18. [18]
  Zhiwen HU , Weixia DONG , Qifu BAO , Ping LI . Low-temperature synthesis of tetragonal BaTiO₃ for piezocatalysis. Chinese Journal of Inorganic Chemistry, 2024, 40(5): 857-866. doi: 10.11862/CJIC.20230462
19. [19]
  Haiyang Zhang , Yanzhao Dong , Haojie Li , Ruili Guo , Zhicheng Zhang , Jiangjiexing Wu . Exploring the Integration of Chemical Engineering Principle Experiment with Cutting-Edge Research Achievements. University Chemistry, 2024, 39(10): 308-313. doi: 10.12461/PKU.DXHX202405035
20. [20]
  Xiaojun Liu , Lang Qin , Yanlei Yu . Dynamic Manipulation of Photonic Bandgaps in Cholesteric Liquid Crystal Microdroplets for Applications. Acta Physico-Chimica Sinica, 2024, 40(5): 2305018-0. doi: 10.3866/PKU.WHXB202305018

Get Citation

PDF

XML

Metrics

PDF Downloads(1)
Abstract views(711)
HTML views(65)

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