Determination of Pesticide Residues in Fruit and Vegetables by High-Performance Liquid Chromatography–Tandem Mass Spectrometry with Multivariate Response Surface Methodology

ABSTRACT

Multivariate response surface methodology optimization using Placket–Burman and Box–Behnken designs were respectively used for the screening and optimization of significant factors for liquid chromatography–tandem mass spectrometry. Consequently, the optimized instrument successfully improved the sample preparation protocol and the method was validated. However, modified QuEChERS dispersive solid phase extraction coupled with ionic liquid-based dispersive liquid–liquid microextraction were used for the determination of multi-pesticide residues in fruit and vegetable samples. The analysed samples were jackfruit, strawberries, cucumber, pears, and carrots. The resulting linearity range (5–400 µg/kg) and regression coefficient (>0.99) results were satisfactory. The 94.2 and 95.8% accuracy (89–138%) and precision (0–25%) results were satisfactory and within the recommended ranges (≤20%) and (70–120%), respectively. The limits of detection (0.01–0.54 µg/kg) and quantitation (0.03–1.79 µg/kg) were excellent. The matrix effects (≤−87%) for all analysed samples were not significant. The estimated measurement uncertainties (≤27%) were within the acceptable range (≤50%). Justifiably, the response surface methodology optimized instrument and sample treatment techniques were reliable and convenient for multi-pesticide residue determination in various fruits and vegetables.

KEYWORDS:

• Dispersive liquid–liquid microextraction
• high-performance liquid chromatography–tandem mass spectrometry
• multivariate response surface methodology
• solid-phase extraction

Additional information

Funding

The Postgraduate Research Project (IPPP) supported this research under the grant no. PG 174-2014B, University of Malaya Kuala Lumpur, Malaysia.