Citation: YANG Xu, LIU Mei-Jiao, LIN Shen, XU Dan, DONG Xiang-Chao. Determination of Tetracycline Residues in Milk by On-line Coupling of Restricted Access Material Solid Phase Extraction with High Performance Liquid Chromatography[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(1): 146-151. doi: 10.11895/j.issn.0253-3820.150443 shu

Determination of Tetracycline Residues in Milk by On-line Coupling of Restricted Access Material Solid Phase Extraction with High Performance Liquid Chromatography

1.
College of Chemistry, Nankai University, Tianjin 300071, China

Corresponding author: DONG Xiang-Chao,
Received Date: 27 May 2015
Available Online: 13 September 2015

A new method has been developed for the determination of tetracycline residues in milk by on-line restricted access material solid phase extraction-HPLC analysis. Restricted accessed poly(styrene-co-divinylbenzene) bonded silica, synthesized by atom transfer radical polymerization, was used as solid phase extraction material in the experiment. This material played both functions of tetracylines extraction and biomacromolecule exclusion. Tetracyclines extracted from milk sample were back-flushed into a reversed phase C₁₈ analytical column and oxytetracycline, tetracycline and chlortetracycline were separated and quantified by HPLC analysis. The exclusion ratio of bovine serum albumin from the restricted access material column was 96.0%, which indicated that the restricted access material had the ability to exclude large biological molecules. The recoveries of three tetracylines in milk samples were 88.3%-101.5% with relative standard deviations <8.0%. The detection limits of 50-80 μg/L and the linear ranges from 0.05 μg/mL to 2.0 μg/mL for the analytes were obtained. The results demonstrated that the method could be used in the determination of tetracycline residues in milk samples with good sensitivity and efficiency.
1. [1]
  1 Kemper N. Ecol. Indic., 2008,8(1):1-13
2. [2]
  2 Daghrir R, Drogui P. Environ. Chem. Lett., 2013,11(3):209-227
3. [3]
  3 P. R. China Bulletin of Ministry of Agriculture, no. 235, Veterinary Drug Maximum Residue Limits in the Food of Animal Origin,2002
4. [4]
  4 U. S. Code of federal regulations, Title 21, Part 556, Tolerances for Residues of New Animal Drugs in Food,2003
5. [5]
  5 Council regulation (EEC) 2377/90, Laying Down a Community Procedure for the Establishment of Maximum Residue Limits Veterinary Medicinal Products in Foodstuffs of Animal Origin, 1990[LM]
6. [6]
  6 Vidal J L M, Aguilera-Luiz M D M, Romero-González R, Frenich A G. J. Agric. Food. Chem., 2009,57(5):1760-1767
7. [7]
  7 Spisso B F, de Araújo Júnior M G, Monteiro M A, Lima A M B, Pereira M U, Luiz R A, Nóbrega A W D. Anal. Chim. Acta, 2009,656(1-2):72-84
8. [8]
  8 T lgyesi L, Békési K, Sharma V K, Fekete J. Meat Science, 2014,96(3):1332-1339
9. [9]
  9 Cinquina A L, Longo F, Anastasi G, Giannetti L, Cozzani R. J. Chromatogr. A, 2003,987(1-2):227-233
10. [10]
  10 SUN Li-Xin. Food Research And Development, 2012,33(9):167-173 孙立新. 食品研究与开发,2012,33(9):167-173
11. [11]
  11 Yang X Q, Yang C X, Yan X P. J. Chromatogr. A, 2013,1304:28-33
12. [12]
  12 Santos S M, Henriques M, Duarte A C, Esteves V I. Talanta, 2007,71(2):731-737
13. [13]
  13 Pastor N N. Maquieira P R. Anal. Bioanal. Chem., 2009,395(4):907-920
14. [14]
  14 Hennion M C. J. Chromatogr. A, 1999,856(1-2):3-54
15. [15]
  15 Mehdinia A, Aziz-Zanjani M O. TrAC, Trends Anal. Chem., 2013,51:13-22
16. [16]
  16 Cassiano N, Lima V, Oliveira R, De Pietro A, Cass Q. Anal. Bioanal. Chem., 2006,384(7):1462-1469
17. [17]
  17 Sadílek P, Satínsky D, Solich P. TrAC, Trends Anal. Chem., 2007,26(5):375-384
18. [18]
  18 Xu W, Su S, Jiang P, Wang H, Dong X, Zhang M. J. Chromatogr. A, 2010,1217(46):7198-7207
19. [19]
  19 Wang Y, Wang Y, Chen L, Wan Q H. J. Magn. Magn. Mater., 2012,324(4):410-417
20. [20]
  20 Barbosa A F, Barbosa V M P, Bettini J, Luccas P O, Figueiredo E C. Talanta, 2015,131:213-220
21. [21]
  21 Beinhauer J, Bian L Q, Fan H, Sebela M, Kukula M, Barrera J A, Schug K A. Anal. Chim. Acta, 2015,858:74-81
22. [22]
  22 Xu D, Dong X, Zhang H, Wang H, Jiang P, Zhang M. J. Sep. Sci., 2012,35(13):1573-1581
23. [23]
  23 Oka H, Ito Y, Matsumoto H. J. Chromatogr. A, 2000,882:109-133
1. [1]
  Junjie Zhang , Yue Wang , Qiuhan Wu , Ruquan Shen , Han Liu , Xinhua Duan . Preparation and Selective Separation of Lightweight Magnetic Molecularly Imprinted Polymers for Trace Tetracycline Detection in Milk. University Chemistry, 2024, 39(5): 251-257. doi: 10.3866/PKU.DXHX202311084
2. [2]
  Shumin Zhang , Yaqi Wang , Zelin Wang , Libo Wang , Changsheng An , Difa Xu . Ultrafast electron transfer at the ZIS_1−x/UCN S-scheme interface enables efficient H₂O₂ photosynthesis coupled with tetracycline degradation. Acta Physico-Chimica Sinica, 2025, 41(11): 100136-0. doi: 10.1016/j.actphy.2025.100136
3. [3]
  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
4. [4]
  Jinwang Wu , Qijing Xie , Chengliang Zhang , Haifeng Shi . Rationally Designed ZnFe_1.2Co_0.8O₄/BiVO₄ S-Scheme Heterojunction with Spin-Polarization for the Elimination of Antibiotic. Acta Physico-Chimica Sinica, 2025, 41(5): 100050-0. doi: 10.1016/j.actphy.2025.100050
5. [5]
  Shijie Li , Ke Rong , Xiaoqin Wang , Chuqi Shen , Fang Yang , Qinghong Zhang . Design of Carbon Quantum Dots/CdS/Ta₃N₅ S-scheme Heterojunction Nanofibers for Efficient Photocatalytic Antibiotic Removal. Acta Physico-Chimica Sinica, 2024, 40(12): 2403005-0. doi: 10.3866/PKU.WHXB202403005
6. [6]
  Deyun Ma , Fenglan Liang , Qingquan Xue , Yanping Liu , Chunqiang Zhuang , Shijie Li . Interfacial engineering of Cd_0.5Zn_0.5S/BiOBr S-scheme heterojunction with oxygen vacancies for effective photocatalytic antibiotic removal. Acta Physico-Chimica Sinica, 2025, 41(12): 100190-0. doi: 10.1016/j.actphy.2025.100190
7. [7]
  Kexin Dong , Chuqi Shen , Ruyu Yan , Yanping Liu , Chunqiang Zhuang , Shijie Li . Integration of Plasmonic Effect and S-Scheme Heterojunction into Ag/Ag₃PO₄/C₃N₅ Photocatalyst for Boosted Photocatalytic Levofloxacin Degradation. Acta Physico-Chimica Sinica, 2024, 40(10): 2310013-0. doi: 10.3866/PKU.WHXB202310013
8. [8]
  Tengyue ZHANG , Jingjing FENG , Zili LIANG , Jia′nan DAI , Jing MA . Optimization of C-doped BiVO₄ performance for tetracycline degradation using response surface methodology-assisted orthogonal experiments. Chinese Journal of Inorganic Chemistry, 2025, 41(12): 2561-2574. doi: 10.11862/CJIC.20250104
9. [9]
  Jianjun LI , Mingjie REN , Lili ZHANG , Lingling ZENG , Huiling WANG , Xiangwu MENG . UV-assisted degradation of tetracycline hydrochloride by MnFe₂O₄@activated carbon activated persulfate. Chinese Journal of Inorganic Chemistry, 2024, 40(10): 1869-1880. doi: 10.11862/CJIC.20240187
10. [10]
  Jiahong WANG , Zekun XU , Tianjiao LU , Jinming HUANG . Performance of N, Mn doped semi-coke activated carbon catalyzed ozone oxidation for the degradation of tetracycline hydrochloride in water. Chinese Journal of Inorganic Chemistry, 2025, 41(12): 2549-2560. doi: 10.11862/CJIC.20250120
11. [11]
  Rui LIU , Xinjun ZHOU , Tao WANG . Photocatalytic degradation performance of tetracycline by MOF-74-Mn/g-C₃N₄ Z-type heterojunction. Chinese Journal of Inorganic Chemistry, 2025, 41(9): 1796-1804. doi: 10.11862/CJIC.20250033
12. [12]
  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
13. [13]
  Jijun Sun , Qianlang Wang , Qian Chen , Quanqin Zhao , Shumei Zhai . The Antibiotic Legion’s Manifesto to Human Allies. University Chemistry, 2025, 40(4): 307-321. doi: 10.12461/PKU.DXHX202405206
14. [14]
  Chengqian Mao , Yanghan Chen , Haotong Bai , Junru Huang , Junpeng Zhuang . Photodimerization of Styrylpyridinium Salt and Its Application in Silk Screen Printing. University Chemistry, 2024, 39(5): 354-362. doi: 10.3866/PKU.DXHX202312014
15. [15]
  Ruoqian Zhang , Chaoqun Mu , Yali Hou , Mingming Zhang . 四苯乙烯基多组分金属有机笼的构筑及其固态发光性能研究. University Chemistry, 2025, 40(8): 277-283. doi: 10.12461/PKU.DXHX202410027
16. [16]
  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
17. [17]
  Fugui XI , Du LI , Zhourui YAN , Hui WANG , Junyu XIANG , Zhiyun DONG . Functionalized zirconium metal-organic frameworks for the removal of tetracycline from water. Chinese Journal of Inorganic Chemistry, 2025, 41(4): 683-694. doi: 10.11862/CJIC.20240291
18. [18]
  Jiahui YU , Jixian DONG , Yutong ZHAO , Fuping ZHAO , Bo GE , Xipeng PU , Dafeng ZHANG . The morphology control and full-spectrum photodegradation tetracycline performance of microwave-hydrothermal synthesized BiVO₄:Yb³⁺,Er³⁺ photocatalyst. Journal of Fuel Chemistry and Technology, 2025, 53(3): 348-359. doi: 10.1016/S1872-5813(24)60514-1
19. [19]
  Chao Liu , Huan Yu , Jiaming Li , Xi Yu , Zhuangzhi Yu , Yuxi Song , Feng Zhang , Qinfang Zhang , Zhigang Zou . 具有光热效应的多级Ti₃C₂/Bi₁₂O₁₇Br₂肖特基异质结简单合成及其太阳能驱动抗生素光降解的研究. Acta Physico-Chimica Sinica, 2025, 41(7): 100075-0. doi: 10.1016/j.actphy.2025.100075
20. [20]
  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

Get Citation

PDF

XML

Metrics

PDF Downloads(0)
Abstract views(708)
HTML views(78)

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