Dispersive liquid-liquid microextraction coupled with microfluidic paper-based analytical device for the determination of organophosphate and carbamate pesticides in the water sample

Anal Sci. 2022 Oct;38(10):1359-1367. doi: 10.1007/s44211-022-00167-7. Epub 2022 Jul 31.

Abstract

A microfluidic paper-based analytical device (µ-PAD) is a promising new technology platform for the development of extremely low-cost sensing devices. However, it has low sensitivity that might not enable to measure maximum allowable concentration of various pollutants in the environment. In this study, a dispersive liquid-liquid microextraction (DLLME) was developed as a preconcentration method to enhance the sensitivity of the µ-PAD for trace analysis of selected pesticides. Four critical parameters (volume of n-hexane and acetone, extraction time, NaCl amount) that affect the efficiency of DLLME have been optimized using response surface methodology. An acceptable mean recovery of 79-97% and 83-93% was observed at 1 µg L-1 and 5 µg L-1 fortification level, respectively, with very good repeatability (2.2-6.01% RSD) and reproducibility (5.60-10.41% RSD). Very high enrichment factors ranging from 317 to 1471 were obtained. The limits of detection for the studied analytes were in the range of 0.18-0.41 µg L-1 which is much lower than the WHO limits of 5-50 µg L-1 for similar category of analytes. Therefore, by coupling DLLME with µ-PAD, a sensitivity that allows to detect environmental threat and also that surpassed most of the previous reports have been achieved in this study. This implies that the preconcentration step has a paramount contribution to address the sensitivity problem associated with µ-PAD.

Keywords: Box–Behnken design; Dispersive liquid–liquid microextraction; Inhibition percent; Microfluidic paper-based analytical device; Pesticide.

MeSH terms

  • Acetone / analysis
  • Carbamates / analysis
  • Liquid Phase Microextraction* / methods
  • Microfluidics
  • Organophosphates / analysis
  • Pesticides* / analysis
  • Reproducibility of Results
  • Sodium Chloride
  • Water
  • Water Pollutants, Chemical* / analysis

Substances

  • Carbamates
  • Organophosphates
  • Pesticides
  • Water Pollutants, Chemical
  • Water
  • Acetone
  • Sodium Chloride