Citation: LIU Xiao-Ting, YU Shan, YUAN Ming, GUO Qiang-Sheng, GONG Can, XU Xu. Determination of Epigoitrin in Radix Isatidis by Solid Phase Extraction-Quantitative Nuclear Magnetic Resonance Spectroscopy[J]. Chinese Journal of Analytical Chemistry, ;2017, 45(7): 1059-1065. doi: 10.11895/j.issn.0253-3820.170115 shu

Determination of Epigoitrin in Radix Isatidis by Solid Phase Extraction-Quantitative Nuclear Magnetic Resonance Spectroscopy

School of Chemical and Environmental Engineering, Shanghai Institute of Technology, Shanghai 201418, China

Received Date: 27 February 2017
Revised Date: 26 May 2017

Fund Project: This work was supported by the National Natural Science Foundation of China (No. 31671928) and Natural Science Foundation of Shanghai, China (No. 15ZR1440800)

The method of quantitative nuclear magnetic resonance spectroscopy (qNMR) for determination of epigoitrin in Radix Isatidis was established based on solid phase extraction (SPE). The twice ultrasonic extraction method using pure water was used for fully extracting epigoitrin in sample, and then the extraction was enriched and concentrated by poly-Sery MCX SPE cartridge. The effect of sample pretreatment and qNMR experimental conditions was investigated. The qNMR experiment conditions were selected using DMSO as solvent, calibrated 2,3,5-triiodobenzoate as internal standard, and P₁(pulse width)=14.1 μs, d₁(pulse delay time)=5 s, N_S(number of scan)=256. The ¹H-NMR peaks of δ 5.365-5.399 (H-7b, d, 1H) of epigoitrin were chosen as the quantitative peaks. Method validation was performed including precision (intra-day precision RSD was 0.5%, and the inter-day precision was 0.8%), linearity (correlation coefficient r>0.9991), LOD (0.05 mg/g, standard curve method) and LOQ (0.19 mg/g, S/N≥150). The recoveries of the SPE-qNMR were 97.4%-101.7%. The result showed that the method was stable, accurate and reliable. With this method the epigoitrin in a real Radix Isatidis was determined to be ＜0.19-1.26 mg/g. SPE combining with qNMR could extend the application field of qNMR, especially in the detection of low-content component in complex samples.
- Quantitative nuclear magnetic resonance,
- Solid phase extraction,
- Epigoitrin,
- Radix Isatidis
1. [1]
2. [2]
3. [3]
4. [4]
5. [5]
6. [6]
7. [7]
8. [8]
9. [9]
10. [10]
11. [11]
12. [12]
13. [13]
14. [14]
15. [15]
16. [16]
17. [17]
18. [18]
19. [19]
20. [20]
21. [21]
22. [22]
23. [23]
24. [24]
25. [25]
26. [26]
27. [27]
28. [28]
29. [29]
30. [30]
31. [31]
32. [32]
33. [33]
34. [34]
35. [35]
36. [36]
37. [37]
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]
  Jinkang Jin , Yidian Sheng , Ping Lu , Zhan Lu . Introducing a Website for Learning Nuclear Magnetic Resonance (NMR) Spectrum Analysis. University Chemistry, 2024, 39(11): 388-396. doi: 10.12461/PKU.DXHX202403054
3. [3]
  Haolin Zhan , Qiyuan Fang , Jiawei Liu , Xiaoqi Shi , Xinyu Chen , Yuqing Huang , Zhong Chen . Noise Reduction of Nuclear Magnetic Resonance Spectroscopy Using Lightweight Deep Neural Networ. Acta Physico-Chimica Sinica, 2025, 41(2): 100017-. doi: 10.3866/PKU.WHXB202310045
4. [4]
  Hao Wu , Zhen Liu , Dachang Bai . ¹H NMR Spectrum of Amide Compounds. University Chemistry, 2024, 39(3): 231-238. doi: 10.3866/PKU.DXHX202309020
5. [5]
  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
6. [6]
  Zhuoming Liang , Ming Chen , Zhiwen Zheng , Kai Chen . Multidimensional Studies on Ketone-Enol Tautomerism of 1,3-Diketones By ¹H NMR. University Chemistry, 2024, 39(7): 361-367. doi: 10.3866/PKU.DXHX202311029
7. [7]
  Lihui Jiang , Wanrong Dong , Hua Yang , Yongqing Xia , Hongjian Peng , Jun Yuan , Xiaoqian Hu , Zihan Zeng , Yingping Zou , Yiming Luo . Study on Extraction of p-Hydroxyacetophenone. University Chemistry, 2024, 39(11): 259-268. doi: 10.12461/PKU.DXHX202402056
8. [8]
  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
9. [9]
  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-. doi: 10.3866/PKU.WHXB202309036
10. [10]
  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
11. [11]
  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
12. [12]
  Fang Niu , Rong Li , Qiaolan Zhang . Analysis of Gas-Solid Adsorption Behavior in Resistive Gas Sensing Process. University Chemistry, 2024, 39(8): 142-148. doi: 10.3866/PKU.DXHX202311102
13. [13]
  Xuan Zhou , Yi Fan , Zhuoqi Jiang , Zhipeng Li , Guowen Yuan , Laiying Zhang , Xu Hou . Liquid Gating Mechanism and Basic Properties Characterization: a New Experimental Design for Interface and Surface Properties in the Chemistry “101 Plan”. University Chemistry, 2024, 39(10): 113-120. doi: 10.12461/PKU.DXHX202407111
14. [14]
  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
15. [15]
  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
16. [16]
  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
17. [17]
  Wei Zhao , Ying Gan , Xihe Bi . Nurturing with Dedication: Springing into Excellence in Chemistry Postgraduate Education at Northeast Normal University. University Chemistry, 2024, 39(6): 29-36. doi: 10.3866/PKU.DXHX202312032
18. [18]
  Mingyang Men , Jinghua Wu , Gaozhan Liu , Jing Zhang , Nini Zhang , Xiayin Yao . 液相法制备硫化物固体电解质及其在全固态锂电池中的应用. Acta Physico-Chimica Sinica, 2025, 41(1): 2309019-. doi: 10.3866/PKU.WHXB202309019
19. [19]
  Min Gu , Huiwen Xiong , Liling Liu , Jilie Kong , Xueen Fang . Rapid Quantitative Detection of Procalcitonin by Microfluidics: An Instrumental Analytical Chemistry Experiment. University Chemistry, 2024, 39(4): 87-93. doi: 10.3866/PKU.DXHX202310120
20. [20]
  Zehua Zhang , Haitao Yu , Yanyu Qi . 多重共振TADF分子的设计策略. Acta Physico-Chimica Sinica, 2025, 41(1): 2309042-. doi: 10.3866/PKU.WHXB202309042

Get Citation

PDF

XML

Metrics

PDF Downloads(4)
Abstract views(718)
HTML views(101)

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