Simultaneous HPLC/UV Detection of Sulfonamides in Milk Using Fabric Phase Sorptive Extraction

Simultaneous HPLC/UV Detection of Sulfonamides in Milk Using Fabric Phase Sorptive Extraction




Sulfonamides, Milk, FPSE, HPLC/UV


The fabric phase sorptive extraction technique was employed for the simultaneous removal of sulfamethazine and sulfamethoxazole in milk. To achieve this, a cotton fabric was coated with a sol-gel solution of polyethylene glycol to serve as a substrate in the adsorption process. The coated and uncoated fabrics were characterized using x-ray energy dispersive spectroscopy and scanning electron microscopy, confirming the effectiveness of the coating procedure. Quantification of the analytes was conducted using high-performance liquid chromatography with ultraviolet detection, with a wavelength of 267 nm. The mobile phase that exhibited the best analytical separation and selectivity for the studied analytes in the presence of the complex milk matrix consisted of acetonitrile and water (30:70 v/v). The results of the evaluation of the removal capacity of sulfonamides were 35.30 % ± 1.09 for sulfamethazine and 42.79 % ± 1.68 for sulfamethoxazole, demonstrating the effectiveness of the adsorbent system and the methodology used in the extraction and detection of these compounds in milk.


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Author Biographies

Glenda Máris Mesquita De Filippis, Universidade Federal de Catalão

PhD student, Dept. of Chemistry, UFCAT, Catalão, GO, Brazil; E-mail:

Luciana Melo Luciana Melo, Universidade Federal de Catalão

Dr. Prof., Dept. of Chemistry, UFCAT, Catalão, GO, Brazil; E-mail:

Edmar Isaias de Melo, Universidade Federal de Uberlândia

Dr. Prof., Dept. of Chemistry, UFU, Monte Carmelo, MG, Brazil; E-mail:


Anthemidis, A., Kazantzi, V., Samanidou, V., Kabir, A., & Furton, K. G. (2016). An automated flow injection

system for metal determination by flame atomic absorption spectrometry involving on-line fabric disk

sorptive extraction technique. Talanta, 156-157, 64–70.

Armentano, A., Summa, S., Magro, S. L., Palermo, C., Nardiello, D., Centonze, D., & Muscarella, M. (2018).

Rapid method for the quantification of 13 sulphonamides in milk by conventional high-performance

liquid chromatography with diode array ultraviolet detection using a column packed with core-shell

particles. Journal of Chromatography A, 1531, 46–52.

Brazilian Health Regulatory Agency. (2019). Normative Instruction No. 51, dated December 19, 2019.

Dost, K., Jones, D. C., & Davidson, G. (2000). Determination of sulfonamides by packed column supercritical

fluid chromatography with atmospheric pressure chemical ionisation mass spectrometric detection.

Analyst, 125, 1243–1247.

Duan, X., Liu, X., Dong, Y., Yang, J., Zhang, J., He, S., Yang, F., Wang, Z., & Dong, Y. (2020). A green

HPLC method for determination of nine sulfonamides in milk and beef, and its greenness assessment

with analytical eco-scale and greenness profile. Journal of AOAC International, 103(4), 1181–1189.

Feng, Y., Hu, X., Zhao, F., & Zeng, B. (2019). Fe3O4/reduced graphene oxide-carbon nanotubes composite

for the magnetic solid-phase extraction and HPLC determination of sulfonamides in milk. Journal

of Separation Science, 42(5), 1058–1066.

Kabir, A., & Furton, K. G. (2014). Fabric Phase Sorptive Extractors (FPSE) (14, 216, 121) United States

Patent and Trademark Office.

Kabir, A., Furton, K. G., & Malik, A. (2013). Innovations in sol-gel microextraction phases for solventfree sample preparation in analytical chemistry. Trends in Analytical Chemistry, 45, 197–218. DOI:

Kabir, A., Hamlet, C., & Malik, A. (2004). Parts per quadrillion level ultra-trace determination of polar

and nonpolar compounds via solvent-free capillary microextraction on surface-bonded sol-gel

polytetrahydrofuran coating and gas chromatography–flame ionization detection. Journal of Chromatography A, 1047(1), 1–13.

Karageorgou, E., Manousi, N., Samanidou, V., Kabir, A., & Furton, K. G. (2016). Fabric phase sorptive

extraction for the fast isolation of sulfonamides residues from raw milk followed by high performance

liquid chromatography with ultraviolet detection. Food Chemistry, 196, 428–436.

Kechagia, M., Samanidou, V., Kabir, A., & Furton, K. G. (2017). P41: HPLC method development and DOI:

validation for the determination of sulfonamides residues in milk samples. Imekofoods [Proceedings].

º Metrology Promoting Harmonization & Standardization in Food & Nutrition. https://www.imeko.


Khaniki, G. R. J. (2007). Chemical contaminants in milk and public health concerns: A review. International

Journal of Dairy Science, 2(2), 104–115.

Kumar, R., Gaurav, Heena, Malik, A. K., Kabir, A., & Furton, K. G. (2014). Efficient analysis of selected

estrogens using fabric phase sorptive extraction and high performance liquid chromatographyfluorescence detection. Journal of Chromatography A, 1359, 16–25. DOI:

Li, Y., Wu, X., Li, Z., Zhong, S., Wang, W., Wang, A., & Chen, J. (2015). Fabrication of CoFe2O4-graphene

nanocomposite and its application in the magnetic solid phase extraction of sulfonamides from milk

samples. Talanta, 144, 1279–1286.

Liao, W., Ning, Y., Zhang, Y., Wang, W., & Wang, A. (2021). Determination of sulfonamides in milk and egg

samples by HPLC with mesoporous polymelamine-formaldehyde as magnetic solid-phase extraction

adsorbent. Journal of Separation Science, 44(24), 4402–4411.

Maggira, M., Deliyanni, E. A., & Samanidou, V. F. (2019). Synthesis of graphene oxide based sponges

and their study as sorbents for sample preparation of cow milk prior to HPLC determination of

sulfonamides. Molecules, 24(11), 2086.

Maldaner, L., Collins, C. H., & Jardim, I. C. S. F. (2010). Fases estacionárias modernas para cromatografia

líquida de alta eficiência em fase reversa. Química Nova, 33(7), 1559–1568.

Manzanares, N. A., Gracia, L. G., & Campaña, A. M. G. (2014). Alternative sample treatments for the

determination of sulfonamides in milk by HPLC with fluorescence detection. Food Chemistry, 143,


Ministry of Agriculture and Livestock. (2011). Normative Instruction No. 62, dated December 29, 2011.

Ministry of Agriculture and Livestock. (2022). Mapa do leite: políticas públicas e privadas para o leite.

Nebot, C., Regal, P., Miranda, J. M., Fente, C., & Cepeda, A. (2013). Rapid method for quantification of nine

sulfonamides in bovine milk using HPLC/MS/MS and without using SPE. Food Chemistry, 141(3),


Oliveira, T. M. A. (2012). Otimização de validação de método analítico para preparo da amostra e determinação simultânea de sulfonamidas em mel [Master’s thesis. Federal University of Maranhão].

Digital Library.

Qi, M., Tu, C., Li, Z., Wang, W., Chen, J., & Wang, A. J. (2018). Determination of sulfonamide residues in

honey and milk by HPLC coupled with novel graphene oxide/polypyrrole foam material-pipette tip

solid phase extraction. Food Analytical Methods, 11, 2885–2896.

Roldán-Pijuán, M., Lucena, R., Cárdenas, S., Valcárcel, M., Kabir, A., & Furton, K. G. (2015). Stir fabric

phase sorptive extraction for the determination of triazine herbicides in environmental waters by

liquid chromatography. Journal of Chromatography A, 1376, 35–45.

Samanidou, V., Galanopoulos, L. D., Kabir, A., & Furton, K. G. (2015). Fast extraction of amphenicols

residues from raw milk using novel fabric phase sorptive extraction followed by high-performance

liquid chromatography-diode array detection. Analytica Chimica Acta, 855, 41–50.

Santos, J. R. M. P. (2015). Desenvolvimento de metodologias para a determinação de resíduos de sulfonamidas

em leite [Specialization Monograph, National Institute of Quality Control in Health of Oswaldo

Cruz Foundation]. Digital Library.

Silva, D. B. C. (2018). Uso de antimicrobianos em propriedades leiteiras do estado de Goiás [Master’s Thesis.

Federal University of Goiás]. Digital Library.


Tolika, E. P., Samanidou, V. F., & Papadoyannis, I. N. (2011). Development and validation of an HPLC

method for the determination of tem sulfonamide residues in milk according to 2002/657/EC.

Journal of Separation Science, 34(14), 1627–1635.

Trombete, F. M., Santos, R. R., & Souza, A. L. R. (2014). Residuos de antibióticos en la leche comercializada

en Brasil: una revisión de los estudios publicados en los últimos años. Revista Chilena de Nutrición,

(2), 191–197.

Wang, Y., Liu, L., Xiao, C., Chen, L., Yang, P., Liu, Q., Wang, J., & Liu, X. (2016). Rapid determination

of trace sulfonamides in milk by graphene oxide-based magnetic solid phase extraction coupled

with HPLC/MS-MS. Food Analytical Methods, 9, 2521–2530.

Wu, Y. L., Li, C., Liu, Y. J., & Shen, J. Z. (2007). Validation method for the determination of sulfonamide

residues in bovine milk by HPLC. Chromatographia, 66, 191–195.

Zhang, J., Li, W., Zhu, W., Yang, Y., Qin, P., Zhou, Q., Lu, M., & Cai, Z. (2019). Mesoporous graphitic carbon

nitride as an efficient sorbent for extraction of sulfonamides prior to HPLC analysis. Microchimica

Acta, 186(279), 1–9.




How to Cite

Filippis, G. M. M. D., Luciana Melo, L. M., & Melo, E. I. de. (2024). Simultaneous HPLC/UV Detection of Sulfonamides in Milk Using Fabric Phase Sorptive Extraction. Semina: Ciências Exatas E Tecnológicas, 45, e49727.