Dispersive liquid-liquid microextraction combined with capillary electrophoresis for simultaneous determination of five fluoroquinolone antibiotics in marine crude drugs, seawater, and seafood samples

Yingying LOU; Guangli ZHAO; Jingyi YAN; Dani SUN; Jinmao YOU; Huiquan XIAO; Huitao LIU; Guisheng LI; Jinhua LI

doi:10.1007/s00343-025-4344-5

Your Location：

Home >

Browse articles >

Dispersive liquid-liquid microextraction combined with capillary electrophoresis for simultaneous determination of five fluoroquinolone antibiotics in marine crude drugs, seawater, and seafood samples

Chemistry | Updated：2026-03-26

- Dispersive liquid-liquid microextraction combined with capillary electrophoresis for simultaneous determination of five fluoroquinolone antibiotics in marine crude drugs, seawater, and seafood samples
- Dispersive liquid-liquid microextraction combined with capillary electrophoresis for simultaneous determination of five fluoroquinolone antibiotics in marine crude drugs, seawater, and seafood samples
- 海洋湖沼学报(英文) 2026年44卷第1期页码：137-149
- Affiliations：
  
  1.College of Chemistry and Chemical Engineering, Shaoxing University, Shaoxing 312000, China
  2.Yantai Institute of Coastal Zone Research, Chinese Academy of Sciences, Yantai 264003, China
  3.School of Pharmacy, Yantai University, Yantai 264005, China
  4.College of Chemistry and Chemical Engineering, Yantai University, Yantai 264005, China
- Author bio：
  
  jmyou6304@163.com
  jhli@yic.ac.cn
- Funds：
  
  the National Natural Science Foundation of China(22176210);the Major Innovation Fund of Shandong Province(2021ZDSYS23)
- DOI：10.1007/s00343-025-4344-5
  中图分类号：
- 收稿：2024-12-18，
  
  录用：2025-03-17，
  
  网络首发：2025-03-31，
  
  纸质出版：2026-01-01
- Accepted：
Scan QR Code
Yingying LOU, Guangli ZHAO, Jingyi YAN, 等. Dispersive liquid-liquid microextraction combined with capillary electrophoresis for simultaneous determination of five fluoroquinolone antibiotics in marine crude drugs, seawater, and seafood samples[J]. 海洋湖沼学报(英文), 2026,44(1):137-149.

LOU Yingying,ZHAO Guangli,YAN Jingyi,et al.Dispersive liquid-liquid microextraction combined with capillary electrophoresis for simultaneous determination of five fluoroquinolone antibiotics in marine crude drugs, seawater, and seafood samples[J].Journal of Oceanology and Limnology,2026,44(01):137-149.
Yingying LOU, Guangli ZHAO, Jingyi YAN, 等. Dispersive liquid-liquid microextraction combined with capillary electrophoresis for simultaneous determination of five fluoroquinolone antibiotics in marine crude drugs, seawater, and seafood samples[J]. 海洋湖沼学报(英文), 2026,44(1):137-149. DOI： 10.1007/s00343-025-4344-5.

LOU Yingying,ZHAO Guangli,YAN Jingyi,et al.Dispersive liquid-liquid microextraction combined with capillary electrophoresis for simultaneous determination of five fluoroquinolone antibiotics in marine crude drugs, seawater, and seafood samples[J].Journal of Oceanology and Limnology,2026,44(01):137-149. DOI： 10.1007/s00343-025-4344-5.

摘要

Abstract

To simultaneously enrich

separate

and determine five fluoroquinolone antibiotics (FQs) in marine crude drugs (MCDs)

seawater and seafood

we conducted this study using vortex assisted dispersed liquid-liquid microextraction (DLLME)

followed by capillary electrophoresis (CE)-UV. A single-variable optimization was employed to examine the factors influencing the separation effect of CE and the extraction efficiency of DLLME

including buffer solution

organic solvent

separation voltage

extractant

dispersant

and sample solution pH. Under the optimal conditions

the baseline separation of the five FQs was achieved within 6 min. The analytical performance of the method was assessed using six types of actual samples

including three MCDs of hippocampus

clam

and kelp

seawater

and two seafood of prawn and pomfret

demonstrating good linearity ranging from 0.1–5 or 0.01–5 μg/mL. The limits of detection (LODs) and limits of quantification (LOQs) for the five FQs in MCDs were 0.002 2–0.029 2 and 0.006 6–0.097 3 μg/mL

respectively. The LODs and LOQs in seawater and seafood were 0.000 9–0.026 2 and 0.002 9–0.087 4 μg/mL

respectively. The matrix effects of this method were evaluated in the hippocampus

seawater

and prawn

and the results show that DLLME could effectively eliminate matrix interference. Satisfactory recovery rates were achieved in all the six tested actual samples. This developed DLLME-CE method was proven simple to operate

accurate and reliable

with high sensitivity

making it suitable for the analysis of multiple antibiotic residues in complex matrices.

关键词

Keywords

references

Ayankojo A G , Reut J , Nguyen V B C et al . 2022 . Advances in detection of antibiotic pollutants in aqueous media using molecular imprinting technique—a review . Biosensors , 12 ( 7 ): 441 , https://doi.org/10.3390/bios12070441 https://doi.org/10.3390/bios12070441 .

Bhatt S , Chatterjee S . 2022 . Fluoroquinolone antibiotics: occurrence, mode of action, resistance, environmental detection, and remediation—a comprehensive review. Environmental Pollution , 315 : 120440 , https://doi.org/10.1016/j.envpol.2022.120440 https://doi.org/10.1016/j.envpol.2022.120440 .

Chen M C , Hsieh M M , Huang X Y . 2024 . Ultrasensitive enantiomeric barbiturate analysis in body fluids through capillary electrophoresis with large volume sample stacking and ultrasound assisted dispersive liquid microextraction. Journal of Chromatography A , 1730 : 465103 , https://doi.org/10.1016/j.chroma.2024.465103 https://doi.org/10.1016/j.chroma.2024.465103 .

European Commission . Document No . SANCO/12571 / 2013 . Guidance Document on Analytical Quality Control and Validation Procedures for Pesticide Residues Analysis in Food and Feed. 2014 . Available online: http://www.eurl-pesticides.eu/library/docs/allcrl/AqcGuidance_Sanco_2013_12571.pdf http://www.eurl-pesticides.eu/library/docs/allcrl/AqcGuidance_Sanco_2013_12571.pdf (accessed on 24 April 2015 ).

Fu X J , Wang Z G , Wang C Y et al . 2016 . Connotation and extension discussion of marine traditional Chinese medicine . World Science and Technology-Modernization of Traditional Chinese Medicine , 18 ( 12 ): 2034 - 2042 , https://doi.org/10.11842/wst.2016.12.002. https://doi.org/10.11842/wst.2016.12.002. (in Chinese with English abstract)

Gao F F , Lu W H , Liu H T et al . 2018 . Dispersive liquid-liquid microextraction of five chlorophenols in water samples followed by determination using capillary electrophoresis . Electrophoresis , 39 ( 19 ): 2431 - 2438 , https://doi.org/10.1002/elps.201800205 https://doi.org/10.1002/elps.201800205 .

Guo Z P , Chen Y . 2024 . Progress of highly reproducible capillary electrophoresis . Chinese Journal of Chromatography , 42 ( 6 ): 544 - 554 , https://doi.org/10.3724/SP.J.1123.2023.12004. https://doi.org/10.3724/SP.J.1123.2023.12004. (in Chinese with English abstract)

Herrera-Herrera A V , Hernández-Borges J , Borges-Miquel T M et al . 2013 . Dispersive liquid-liquid microextraction combined with ultra-high performance liquid chromatography for the simultaneous determination of 25 sulfonamide and quinolone antibiotics in water samples . Journal of Pharmaceutical and Biomedical Analysis , 75 : 130 - 137 , https://doi.org/10.1016/j.jpba.2012.11.026 https://doi.org/10.1016/j.jpba.2012.11.026 .

Hong J W , Liu X M , Yang X Y et al . 2022 . Ionic liquid-based dispersive liquid-liquid microextraction followed by magnetic solid-phase extraction for determination of quinolones . Microchimica Acta , 189 ( 1 ): 8 , https://doi.org/10.1007/s00604-021-05077-5 https://doi.org/10.1007/s00604-021-05077-5 .

Kaale E , Höllein L , Holzgrabe U . 2015 . Development and validation of a generic stability-indicating MEEKC method for five fluoroquinolone antibiotics . Electrophoresis , 36 ( 21-22 ): 2736 - 2744 , https://doi.org/10.1002/elps.201500025 https://doi.org/10.1002/elps.201500025 .

Liu J Y , Lu W H , Liu H T et al . 2016 . Dispersive liquid-liquid microextraction for four phenolic environmental estrogens in water samples followed by determination using capillary electrophoresis . Electrophoresis , 37 ( 19 ): 2502 - 2508 , https://doi.org/10.1002/elps.201500519 https://doi.org/10.1002/elps.201500519 .

Low K , Chai L , Lee C et al . 2021 . Prevalence and risk assessment of antibiotics in riverine estuarine waters of Larut and Sangga Besar River, Perak . Journal of Oceanology and Limnology , 39 ( 1 ): 122 - 134 , https://doi.org/10.1007/s00343-020-9246-y https://doi.org/10.1007/s00343-020-9246-y .

Ma S Y , Yang S X , Song Z H et al . 2020 . A twin enrichment method based on dispersive liquid-liquid microextraction and field-amplified sample injection for the simultaneous determination of sulfonamides . Analyst , 145 ( 5 ): 1825 - 1832 , https://doi.org/10.1039/c9an02127b https://doi.org/10.1039/c9an02127b .

Ma T , Li Z , Jia Q et al . 2016 . Ultrasound-assisted temperature-controlled ionic liquid emulsification microextraction coupled with capillary electrophoresis for the determination of parabens in personal care products . Electrophoresis , 37 ( 12 ): 1624 - 1631 , https://doi.org/10.1002/elps.201500533 https://doi.org/10.1002/elps.201500533 .

Martínez-Pérez-Cejuela H , Benavente F , Simó-Alfonso E F et al . 2021 . A hybrid nano-MOF/polymer material for trace analysis of fluoroquinolones in complex matrices at microscale by on-line solid-phase extraction capillary electrophoresis. Talanta , 233 : 122529 , https://doi.org/10.1016/j.talanta.2021.122529 https://doi.org/10.1016/j.talanta.2021.122529 .

Okoye C O , Nyaruaba R , Ita R E et al . 2022 . Antibiotic resistance in the aquatic environment: analytical techniques and interactive impact of emerging contaminants. Environmental Toxicology and Pharmacology , 96 : 103995 , https://doi.org/10.1016/j.etap.2022.103995 https://doi.org/10.1016/j.etap.2022.103995 .

Pacheco-Fernández I , González-Martín R , e Silva F A et al . 2021 . Insights into coacervative and dispersive liquid-phase microextraction strategies with hydrophilic media—a review . Analytica Chimica Acta , 1143 : 225 - 249 , https://doi.org/10.1016/j.aca.2020.08.022 https://doi.org/10.1016/j.aca.2020.08.022 .

Papon N , Copp B R , Courdavault V . 2022 . Marine drugs: biology, pipelines, current and future prospects for pro duction. Biotechnology Advances , 54 : 107871 , https://doi.org/10.1016/j.biotechadv.2021.107871 https://doi.org/10.1016/j.biotechadv.2021.107871 .

Pu X Y , Wang X , Liu Y P et al . 2023 . A novel deep eutectic solvent-based ultrasound-assisted dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography for the determination of quinolones in environmental water samples. Microchemical Journal , 195 : 109374 , https://doi.org/10.1016/j.microc.2023.109374 https://doi.org/10.1016/j.microc.2023.109374 .

Qiao L Z , Tao Y , Yao W et al . 2022 . A magnetic ionic liquid based vortex-assisted dispersive liquid-liquid microextraction coupled with back-extraction for the enrichment of fluoroquinolone antibiotics. Journal of Pharmaceutical and Biomedical Analysis , 219 : 114903 , https://doi.org/10.1016/j.jpba.2022.114903 https://doi.org/10.1016/j.jpba.2022.114903 .

Raposo F , Barceló D . 2021 . Challenges and strategies of matrix effects using chromatography-mass spectrometry: an overview from research versus regulatory viewpoints. TrAC Trends in Analytical Chemistry , 134 : 116068 , https://doi.org/10.1016/j.trac.2020.116068 https://doi.org/10.1016/j.trac.2020.116068 .

Saraji M , Bidgoli A A H . 2010 . Dispersive liquid-liquid microextraction using a surfactant as disperser agent . Analytical and Bioanalytical Chemistry , 397 ( 7 ): 3107 - 3115 , https://doi.org/10.1007/s00216-010-3894-2 https://doi.org/10.1007/s00216-010-3894-2 .

Shao Y C , Wen Y L , Zhao X Y et al . 2024 . Annual review of capillary electrophoresis technology in 2023 . Chinese Journal of Chromatography , 42 ( 5 ): 401 - 409 , https://doi.org/10.3724/SP.J.1123.2024.02007. https://doi.org/10.3724/SP.J.1123.2024.02007. (in Chinese with English abstract)

Wang G N , Feng C , Zhang H C et al . 2015 . Determination of fluoroquinolone drugs in meat by ionic-liquid-based dispersive liquid-liquid microextraction-high performance liquid chromatography . Analytical Methods , 7 ( 3 ): 1046 - 1052 , https://doi.org/10.1039/c4ay02383h https://doi.org/10.1039/c4ay02383h .

Wang Y X , Li J H , Sun D N et al . 2021 . Strategies of dispersive liquid-liquid microextraction for coastal zone environmental pollutant determination. Journal of Chromatography A , 1658 : 462615 , https://doi.org/10.1016/j.chroma.2021.462615 https://doi.org/10.1016/j.chroma.2021.462615 .

Wang Z R , Hsieh M M . 2020 . Ultrasound-assisted dispersive liquid-liquid microextraction coupled with field-amplified capillary electrophoresis for sensitive and quantitative determination of fluoxetine and norfluoxetine enantiomers in biological fluids . Analytical and Bioanalytical Chemistry , 412 ( 21 ): 5113 - 5123 , https://doi.org/10.1007/s00216-020-02441-x https://doi.org/10.1007/s00216-020-02441-x .

Wei D , Guo M , Zhang J . 2020 . Determination of 10 fluoroquinolones residues in aquatic products by accelerated solvent extraction, magnetic solid-phase extraction, and high-performance liquid chromatography-tandem mass spectrometry . Chinese Journal of Chromatography , 38 ( 12 ): 1413 - 1422 , https://doi.org/10.3724/SP.J.1123.2020.05002. https://doi.org/10.3724/SP.J.1123.2020.05002. (in Chinese with English abstract)

Wen L L , Song J M , Li X G et al . 2023 . Sample pretreatment and determination of fluoroquinolone antibiotics in marine environments . Marine Sciences , 47 ( 9 ): 103 - 118 , https://doi.org/10.11759/hykx20230208001. https://doi.org/10.11759/hykx20230208001. (in Chinese with English abstract)

Yang L , Zhao F K , Yen H et al . 2024 . Urbanization and land use regulate soil vulnerability to antibiotic contamination in urban green spaces. Journal of Hazardous Materials , 465 : 133363 , https://doi.org/10.1016/j.jhazmat.2023.133363 https://doi.org/10.1016/j.jhazmat.2023.133363 .

Yu H , Wang Z H , Wu R et al . 2019 . Water-dispersible pH/thermo dual-responsive microporous polymeric microspheres as adsorbent for dispersive solid-phase extraction of fluoroquinolones from environmental water samples and food samples . Journal of Chromatography A , 1601 : 27 - 34 , https://doi.org/10.1016/j.chroma.2019.05.004 https://doi.org/10.1016/j.chroma.2019.05.004 .

Zeng L , Armani A , Wen J et al . 2019 . Molecular identification of seahorse and pipefish species sold as dried seafood in China: a market-based survey to highlight the actual needs for a proper trade . Food Control , 103 : 175 - 181 , https://doi.org/10.1016/j.foodcont.2019.04.007 https://doi.org/10.1016/j.foodcont.2019.04.007 .

Zhang X H , Deng Y , Zhao M Z et al . 2018 . Highly-sensitive detection of eight typical fluoroquinolone antibiotics by capillary electrophoresis-mass spectroscopy coupled with immunoaffinity extraction . RSC Advances , 8 ( 8 ): 4063 - 4071 , https://doi.org/10.1039/c7ra12557g https://doi.org/10.1039/c7ra12557g .

Zhao F K , Yang L , Tang J F et al . 2023 . Urbanization-land-use interactions predict antibiotic contamination in soil across urban-rural gradients. Science of the Total Environment , 867 : 161493 , https://doi.org/10.1016/j.scitotenv.2023.161493 https://doi.org/10.1016/j.scitotenv.2023.161493 .

Zhong X H , Jiang X Y , He H J et al . 2023 . Application of sequential extraction for analyzing source and sink of uranium in Huanghe River sediments, China . Journal of Oceanology and Limnology , 41 ( 3 ): 936 - 946 , https://doi.org/10.1007/s00343-022-1410-0 https://doi.org/10.1007/s00343-022-1410-0 .

Zhu X M , Zhao C Y , Liu J et al . 2022 . Determination of quinolone antibiotics in honey by pH-induced natural deep eutectic solvent combined with vortex-assisted dispersive liquid-liquid microextraction . Analytical Methods , 14 ( 43 ): 4377 - 4385 , https://doi.org/10.1039/d2ay01172g https://doi.org/10.1039/d2ay01172g .

浏览量

Downloads

CSCD

文章被引用时，请邮件提醒。

Submit

工具集

关联资源

Interlinked water and sediment microplastics in the Laizhou Bay of China

Microplastics in the seawater of the Beibu Gulf, the northern South China Sea: occurrence, sources, and ecological risk

Effects of inorganic nutrients and environmental factors on the removal of n-propylbenzene and isopropylbenzene in seawater by cryptophytes Rhinomonas reticulata S6A

Environmental characteristics of trace metals in seawater from the Ninety East Ridge in the Indian Ocean