Citation: LIU Peiyong, ZHANG Hui, MI Zhijin, ZHANG Liangcheng, ZHANG Guangren. Determination of 11 sulfonamides in pork by two-step liquid-liquid extraction-solid phase extraction purification coupled with high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2019, 37(10): 1098-1104. doi: 10.3724/SP.J.1123.2019.04005 shu

Determination of 11 sulfonamides in pork by two-step liquid-liquid extraction-solid phase extraction purification coupled with high performance liquid chromatography-tandem mass spectrometry

Dazhou Food and Drug Inspection Institute, Dazhou 635000, China

Received Date: 2 April 2019

A method based on two-step liquid-liquid extraction-solid phase extraction purification coupled with high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of 11 common sulfonamides in pork. The samples were extracted first with ethyl acetate containing 2%(v/v) formic acid and then with acetone for the second step. The supernatant was degreased with n-hexane and cleaned using an Oasis MCX SPE column. Finally, nitrogen was blown over the obtained mixture, and the mixture was filtered for conducting HPLC-MS/MS analysis. The sulfonamides were detected in the multiple reaction monitoring positive ion mode, and quantification was performed by employing the external standard method with matrix calibration curves. All the 11 sulfonamides demonstrated good linearity in the range of 20-400 μg/L, with the correlation coefficient (r²) higher than 0.99. The limits of detection (LODs; S/N=3) and limits of quantification (LOQs; S/N=10) were found to be in the ranges of 0.1-1.0 μg/kg and 0.2-3.0 μg/kg, respectively. Furthermore, the results indicated that the average recoveries of the 11 sulfonamides ranged from 79.3% to 105.5% at three spiked levels of 50, 100, and 200 μg/kg, with the relative standard deviations (RSDs) in the range of 1.3%-11.6% (n=6). This method showed higher extraction efficiency than the one-step liquid-liquid extraction, and the detection sensitivity was highly improved.
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]
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]
  Siwei Hou , Yaxin Niu , Guanglu Zhang , Yanmei Yang , Xu Wang , Zhenzhen Chen . Application of Solid-Phase Microextraction and Mass Spectrometry in Environmental Detection. University Chemistry, 2026, 41(3): 297-306. doi: 10.12461/PKU.DXHX202504078
3. [3]
  Haiyuan Wang , Xiaoning Jin , Yajing Sun , Zhen Zhang , Wentao Zhao , Yi Li . Practical Exploration of High-Performance Liquid Chromatography Experiment Teaching Reform Empowered by Artificial Intelligence. University Chemistry, 2026, 41(4): 45-51. doi: 10.12461/PKU.DXHX202505076
4. [4]
  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
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]
  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
7. [7]
  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
8. [8]
  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
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): 100013-0. doi: 10.3866/PKU.WHXB202309036
10. [10]
  Yiru Wang , Chanzi Ruan , Juanjuan Song , Yongxian Fan , Dongcheng Liu , Yanping Ren , Xiuqiong Zeng , Faqiong Zhao , Wenwei Zhang , Mei Shi , Min Hu , Wan Li , Xiuyun Wang , Weihong Li , Xiaohang Qiu , Yong Fan , Jianrong Zhang , Shuyong Zhang . Solid-Liquid Separation and Suggestions on the Operation Standards (I): Decantation and Centrifugation with Centrifuge Operation. University Chemistry, 2026, 41(3): 122-129. doi: 10.12461/PKU.DXHX202507037
11. [11]
  Yiru Wang , Zhiqiang Dong , Juanjuan Song , Yongxian Fan , Dongcheng Liu , Yanping Ren , Xiuqiong Zeng , Faqiong Zhao , Wenwei Zhang , Mei Shi , Min Hu , Wan Li , Xiuyun Wang , Weihong Li , Xiaohang Qiu , Yong Fan , Jianrong Zhang , Shuyong Zhang . Solid-Liquid Separation and Suggestions on the Operation Standards (II): Gravity Filtration and Vacuum Filtration with Vacuum Pump Operation. University Chemistry, 2026, 41(3): 130-142. doi: 10.12461/PKU.DXHX202507042
12. [12]
  Heng Chen , Longhui Nie , Kai Xu , Yiqiong Yang , Caihong Fang . Remarkable Photocatalytic H₂O₂ Production Efficiency over Ultrathin g-C₃N₄ Nanosheet with Large Surface Area and Enhanced Crystallinity by Two-Step Calcination. Acta Physico-Chimica Sinica, 2024, 40(11): 2406019-0. doi: 10.3866/PKU.WHXB202406019
13. [13]
  Yutong Dong , Huiling Xu , Yucheng Zhao , Zexin Zhang , Ying Wang . The Hidden World of Surface Tension and Droplets. University Chemistry, 2024, 39(6): 357-365. doi: 10.3866/PKU.DXHX202312022
14. [14]
  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
15. [15]
  Yujing Chen , Hongqun Ouyang , Dan Zhao , Yanyan Chu , Zhengping Qiao . Recommendations for the Content and Instruction of the Physical Chemistry Experiment “Construction of Ternary Liquid-Liquid Phase Diagrams”. University Chemistry, 2025, 40(7): 359-366. doi: 10.12461/PKU.DXHX202409120
16. [16]
  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
17. [17]
  Yongqing Kuang , Jie Liu , Jianjun Feng , Wen Yang , Shuanglian Cai , Ling Shi . Experimental Design for the Two-Step Synthesis of Paracetamol from 4-Hydroxyacetophenone. University Chemistry, 2024, 39(8): 331-337. doi: 10.12461/PKU.DXHX202403012
18. [18]
  Jiandong Liu , Xin Li , Daxiong Wu , Huaping Wang , Junda Huang , Jianmin Ma . Anion-Acceptor Electrolyte Additive Strategy for Optimizing Electrolyte Solvation Characteristics and Electrode Electrolyte Interphases for Li||NCM811 Battery. Acta Physico-Chimica Sinica, 2024, 40(6): 2306039-0. doi: 10.3866/PKU.WHXB202306039
19. [19]
  Feiya Cao , Qixin Wang , Pu Li , Zhirong Xing , Ziyu Song , Heng Zhang , Zhibin Zhou , Wenfang Feng . Magnesium-Ion Conducting Electrolyte Based on Grignard Reaction: Synthesis and Properties. University Chemistry, 2024, 39(3): 359-368. doi: 10.3866/PKU.DXHX202308094
20. [20]
  Hao Chen , Dongyue Yang , Gang Huang , Xinbo Zhang . Progress on Liquid Organic Electrolytes of Li-O₂ Batteries. Acta Physico-Chimica Sinica, 2024, 40(7): 2305059-0. doi: 10.3866/PKU.WHXB202305059

Get Citation

PDF

XML

Metrics

PDF Downloads(6)
Abstract views(535)
HTML views(52)

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