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Rapid determination of sulfonamide residues in pork by surface-modified hydrophilic electrospun nanofibrous membrane solid-phase extraction combined with ultra-performance liquid chromatography

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Abstract

This study aimed to rapidly determine 13 representative sulfonamide (SA) residues in pork by using a surface-modified hydrophilic polystyrene sulfonic acid (PSSA) electrospun nanofibrous membrane as the solid-phase extraction (SPE) pretreatment sorbent, followed by ultra-performance liquid chromatography (UPLC) analysis. The highly hydrophilic nature of PSSA nanofibrous membrane created by vacuum plasma treatment was characterized using Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), water contact angle, and X-ray photoelectron spectroscopy (XPS) measurements. In the pretreatment procedures, 13 SA standards, which were spiked in the fatty pork samples, were extracted, enriched, and purified by the SPE procedure based on the principle of ion exchange with the sulfonic groups on the PSSA chains. Under the optimized conditions, the calibration curves of 13 SA compounds showed good linearities with correlation coefficients (r) of more than 0.99 in the range of 50.0–200 μg kg−1. The mean recoveries of 13 SAs at the spiked concentrations of 50, 100, and 200 μg kg−1 were in the range of 70.3–92.5 % with average RSDs (n = 6) of less than 15 % (except for sulfacetamide, 56.9–61.6 %). Compared with other pretreatment methods reported previously, less organic solvent (especially without degreasing the extract with n-hexane) was used in this time-saving SPE procedure, which avoids the possibility of emulsification and therefore enhances the recoveries. The developed and validated analysis method was sensitive, accurate, rapid, convenient, environmentally friendly, and was successfully applied for the detection of 13 SA residues in commercially available pork samples.

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Abbreviations

BE:

Binding energy

DMF:

N,N-dimethylformamide

EDTA:

Ethylenediaminetetraacetic acid

FE-SEM:

Field emission scanning electron microscopy

FT-IR:

Fourier transform infrared spectroscopy

HLB:

Hydrophilic-lipophilic balance

HPLC:

High-performance liquid chromatography

LOD:

Limit of detection

LOQ:

Limit of quantitation

MCX:

Mixed-mode cation exchange

MIP:

Molecularly imprinted polymer

MRL:

Maximum residue limit

MSPD:

Matrix solid-phase dispersion

MWCNT:

Multi-walled carbon nanotube

PP:

Polypropylene

PS:

Polystyrene

PSSA:

Polystyrene sulfonic acid

QC:

Quality control

SFA:

Sulfacetamide

SA:

Sulfonamide

SDM:

Sulfadimethoxine

SIZ:

Sulfisoxazole

SM1 :

Sulfamerazine

SM2 :

Sulfamethazine

SML:

Sulfabenzamide

SMM:

Sulfamonomethoxine

SMP:

Sulfamethoxypyridazine

SMZ:

Sulfamethoxazole

SP:

Sulfapyridine

SPD:

Sulfachlorpyridazine

SPE:

Solid-phase extraction

SPP:

Sulfaphenazole

SX:

Sulfamoxol

THF:

Tetrahydrofuran

UPLC:

Ultra-performance liquid chromatography

XPS:

X-ray photoelectron spectroscopy

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Acknowledgements

The project was sponsored by the Jiangsu Province Science Foundation for Youths (BK20130644) and the Fundamental Research Funds for the Central Universities (JKQZ2013006). Dr. Rong Chen would also like to acknowledge the China Scholarship Council (CSC 201407060048) for granting a scholarship that enabled her to pursue this work at National University of Singapore, Singapore.

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Authors and Affiliations

  1. Department of Analytical Chemistry, School of Science, China Pharmaceutical University, Nanjing, Jiangsu, 211198, China

    Rong Chen, Yingying Yang, Yue Li, Yong Lu & Weiyang Shen

  2. Center of Nanofibers & Nanotechnology, Department of Mechanical Engineering, National University of Singapore, 2 Engineering Drive 3, Singapore, 117576, Singapore

    Rong Chen, Lingling Tian & Seeram Ramakrishna

  3. Key Laboratory of Drug Quality Control and Pharmacovigilance (Ministry of Education), China Pharmaceutical University, 24 Tongjiaxiang, Nanjing, Jiangsu, 210009, China

    Rong Chen & Weiyang Shen

  4. Jiangsu Quality Inspection and Testing Centre for Animal Products, Nanjing, Jiangsu, 210036, China

    Bin Qu

  5. Guangdong-Hongkong-Macau Institute of CNS Regeneration (GHMICR), Jinan University, Guangzhou, Guangdong, 510632, China

    Seeram Ramakrishna

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  1. Rong Chen
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Chen, R., Yang, Y., Qu, B. et al. Rapid determination of sulfonamide residues in pork by surface-modified hydrophilic electrospun nanofibrous membrane solid-phase extraction combined with ultra-performance liquid chromatography. Anal Bioanal Chem 408, 5499–5511 (2016). https://doi.org/10.1007/s00216-016-9648-z

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