Development of headspace solid-phase microextraction method for the analysis of pesticide residues in fruit and vegetable samples using OFAT design

  • Lukman Bola Abdulra’uf
  • Amudalat Ranti Lawal
  • Guan Huat Tan
Keywords: Univariate design, Simple lattice design, design of experiment, GC-MS, HS-SPME


A headspace solid-phase microextraction (HS-SPME) method was developed as a preliminary investigation using univariate approach for the analysis of 14 multiclass pesticide residues in fruits and vegetable samples. The gas chromatography mass spectrometry parameters (desorption temperature and time, column flow rate, interface temperature) and solid phase microextraction parameters (fiber coating type, extraction temperature and time, pH, salt addition, stirring rate, dilution factor, organic solvent type and amount) were all investigated and optimized. The optimum values for the optimized parameters are as follows: Injection Temperature, 270 °C; Interface temperature, 300 °C; Column flow rate, 1.3 mL/min; Fiber coating, PDMS/DVB; Extraction time, 30 mins; Extraction temperature, 60 °C; Stirring rate, 300 rpm; Salt addition, 10% (v/w) NaCl; pH, 7; Desorption time, 7 min; Desorption temperature, 270°C; Organic solvent 3 % (methanol/acetone, 21:79%). The optimization of the mixture of organic solvents was optimized using design of experiment (DOE) with simplex lattice, designed using Minitab Statistical Software®. The developed method was then applied to the analysis of samples of apple, tomato, broccoli, lettuce, grape, cucumber, cabbage and pear. The investigated pesticides were found to be below the maximum residue levels, while some were not found. This shows that the fruit and vegetable samples are safe for consumption and do not pose any health risk for consumers.

Keywords: Univariate design, Simple lattice design, design of experiment, GC-MS, HS-SPME


Journal Identifiers

eISSN: 2659-1502
print ISSN: 1119-8362