Fast extraction of amphenicols residues from raw milk using novel fabric phase sorptive extraction followed by high-performance liquid chromatography-diode array detection

Anal Chim Acta. 2015 Jan 15;855:41-50. doi: 10.1016/j.aca.2014.11.036. Epub 2014 Dec 3.


A simple, sensitive, reliable, and fast analytical method was developed for the simultaneous determination of amphenicols residues in raw milk by combining fabric phase sorptive extraction (FPSE) and high-performance liquid chromatography-diode array detection. FPSE, a new generation green sample preparation technique, efficiently incorporates the advanced and tunable material properties of sol-gel derived microextraction sorbents with the rich surface chemistry of a cellulose fabric substrate, resulting in a flexible, highly sensitive, and fast microextraction device capable of extracting target analytes directly from complicated sample matrices. Due to the strong chemical bonding between the sol-gel sorbent and substrate, the microextraction device demonstrates a very high chemical and solvent stability. Therefore, any organic solvent/solvent mixture can be used as the eluent/back-extraction solvent. Herein, a highly polar polymer coated FPSE media was created using short-chain poly(ethylene glycol) (PEG) and the applicability of this novel microextraction device to extract highly polar amphenicol antibiotics from raw milk was investigated. Due to the intense affinity of amphenicols towards the strongly polar sol-gel PEG-coated FPSE device, absolute recovery of the selected antibiotics residues were found to be 44% for thiamphenicol, 66.4% for florfenicol, and 81.4% for chloramphenicol. The developed method was validated in terms of sensitivity, linearity, accuracy, precision, and selectivity according to European Decision 657/2002/EC. Decision limit (CCα) values were 52.49 μg kg(-1) for thiamphenicol, 55.23 μg kg(-1) for florfenicol, and 53.8 μg kg(-1) for chloramphenicol, while the corresponding results for detection capability (CCβ) were 56.8 μg kg(-1), 58.99 μg kg(-1), and 55.9 μg kg(-1), respectively.

Keywords: Amphenicols; Fabric phase sorptive extraction (FPSE); Milk; Sample preparation; Sorptive extraction.

MeSH terms

  • Animals
  • Cellulose / chemistry
  • Chemical Fractionation / instrumentation
  • Chemical Fractionation / methods*
  • Chloramphenicol / analysis*
  • Chloramphenicol / chemistry
  • Chloramphenicol / isolation & purification*
  • Chromatography, High Pressure Liquid
  • Drug Residues / analysis*
  • Drug Residues / chemistry
  • Drug Residues / isolation & purification*
  • Hydrophobic and Hydrophilic Interactions
  • Milk / chemistry*
  • Octanols / chemistry
  • Polyethylene Glycols / chemistry
  • Time Factors
  • Water / chemistry


  • Octanols
  • Water
  • Polyethylene Glycols
  • Chloramphenicol
  • Cellulose