Pesticides are widely applied to prevent unwanted pests from attacking crops and livestock which led to their access into the environment. Overuses of pesticides in environment are presence of pesticide residues and their metabolites that are causing serious detrimental effects on human health and all other living organisms. Several severe diseases (Cancer, chronic obstructive pulmonary disease, birth defects, infertility) and more damages of human health are associated with the exposure of pesticides. The maximum residue limits for pesticides have been regulated by the Codex Alimentarius Commission and European Union to protect human health. Thus, monitoring these compounds is extremely important to ensure that only permitted levels of pesticide are consumed. To date, several techniques have been developed for pesticide detection, from conventional analytical to advanced detection techniques. The conventional analytical methods are gas chromatography and high performance liquid chromatography coupled with various detectors involved a sample preparation step prior to further analysis. Advanced detection methods refer to the sensors development such as electrochemical, optical, piezoelectric and molecular imprinted polymer. In this review, we summarized and explained the available analytical and advanced methods for determination of pesticides compound in environment and foodstuffs. Also, pesticides classification and its toxicity, and available extraction methods are briefly discussed.

A review of extraction, analytical and advanced methods for determination of pesticides in environment and foodstuffs

Magnetic solid-phase extraction (MSPE), an emerging sample pretreatment technique, has received much attention because of its environment friendliness, rapid separation process, excellent adsorption efficiency, and easily automated assay. This paper reviews the nature of MSPE, and the types and preparation of magnetic adsorbents. It also discusses recent application of MSPE to the analysis of trace contaminants in food samples, such as pesticides and veterinary drug residuals, polymer additives, and heavy metals ions. The future development trends of MSPE in food safety analysis are also investigated. High efficiency, low cost, and environmental-friendly food safety detection techniques are expected with the application of MSPE.

Recent application of magnetic solid phase extraction for food safety analysis

Dispersive solid phase microextraction (DSPME) as a prepossessing solid phase microextraction (SPME) technique has been recently considered for the extraction, clean up, and preconcentration of different analytes in real samples. In this review, the advantages and disadvantages of DSPME against SPME are compared based on the practical procedure and their applications. Theory of DSPME is studied to determine the effective factors in the extraction recovery of analytes. Types of DSPME procedure, method limitations, and extensions are discussed to remove these constraints. Moreover, sorbent dispersion procedures in the sample solution and sorbent separation methods from the sample solution are also reviewed and compared.

Dispersive solid phase microextraction

Advances in the area of sample preparation are significant and have been growing significantly in recent years. This initial step of the analysis is essential and must be carried out properly, consisting of a complicated procedure with multiple stages. Consequently, it corresponds to a potential source of errors and will determine, at the end of the process, either a satisfactory result or a fail. One of the advances in this field includes the miniaturization of extraction techniques based on the conventional sample preparation procedures such as liquid-liquid extraction and solid-phase extraction. These modern techniques have gained prominence in the face of traditional methods since they minimize the consumption of organic solvents and the sample volume. As another feature, it is possible to reuse the sorbents, and its coupling to chromatographic systems might be automated. The review will emphasize the main techniques based on liquid-phase microextraction, as well as those based upon the use of sorbents. The first group includes currently popular techniques such as single drop microextraction, hollow fiber liquid-phase microextraction, and dispersive liquid-liquid microextraction. In the second group, solid-phase microextraction techniques such as in-tube solid-phase microextraction, stir bar sorptive extraction, dispersive solid-phase extraction, dispersive micro solid-phase microextraction, and microextraction by packed sorbent are highlighted. These approaches, in common, aim the determination of analytes at low concentrations in complex matrices. This article describes some characteristics, recent advances, and trends on miniaturized sample preparation techniques, as well as their current applications in food, environmental, and bioanalysis fields.

Recent advances and trends in miniaturized sample preparation techniques

This paper reviews the recent advances of ionic liquids (ILs) in sample preparation from more than 100 works mainly in last five years, including liquid-liquid microextraction, solid-phase extraction, solid-phase microextraction, stir bar or stir cake sorptive extraction. ILs, polymer of ILs and their composites with molecular imprinted polymer, carbon nanotubes, graphene oxide and magnetic materials have been explored as promising sorbents for inorganic or organic pollutants, majorly relying on the affinity of ILs with the target. The improved sensitivity and selectivity towards different types of analytes were displayed, attributed from various mechanism of ILs-based extraction materials including π-π, ion-exchange, hydrogen bond, dipole-dipole, electrostatic, hydrophobic and hydrophilic interactions. The prospects of ILs for sample preparation were also presented, which can offer an outlook for the further applications of ILs.

Recent advances of ionic liquids in sample preparation

Magnetic mixed hemimicelles dispersive solid-phase extraction based on ionic liquid-coated attapulgite/polyaniline-polypyrrole/Fe3O4 nanocomposites for determination of acaricides in fruit juice prior to high-performance liquid chromatography-diode array detection.

In this work, a novel extraction technique based on the effervescence-assisted dispersion and magnetic recovery of attapulgite/polypyrrole sorbents was developed for determining the concentrations of five pyrethroids in honey samples. The magnetic nanoparticles were synthesized by a one-pot method. Several experimental parameters that affected the extraction efficiency, including the dispersion conditions, pH, ionic strength, and desorption conditions, were investigated. Under optimal conditions, the calibration curves for the five pyrethroids in honey samples exhibited good linearity, with r2 values ranging from 0.9979 to 0.9990. The limits of detection varied between 0.21 and 0.34 µg/L. Satisfactory recoveries of 81.42-106.73% with intra- and interday relative standard deviations of less than 6.94 and 10.89%, respectively, were obtained. Moreover, the sorbents exhibited acceptable batch-to-batch repeatability in the range of 5.06-15.01%, and each sorbent could be reused for up to four extraction cycles without a significant loss in the extraction recovery.

Preparation of magnetic attapulgite/polypyrrole nanocomposites for magnetic effervescence‐assisted dispersive solid‐phase extraction of pyrethroids from honey samples

A dispersive magnetic solid phase microextraction based on ionic liquid-coated and cyclodextrin-functionalized magnetic core dendrimer nanocomposites for the determination of pyrethroids in juice samples.

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Magnetic mixed hemimicelles dispersive solid-phase extraction based on ionic liquid-coated attapulgite/polyaniline-polypyrrole/Fe3O4 nanocomposites for determination of acaricides in fruit juice prior to high-performance liquid chromatography-diode array detection.

Preparation of magnetic attapulgite/polypyrrole nanocomposites for magnetic effervescence‐assisted dispersive solid‐phase extraction of pyrethroids from honey samples

A dispersive magnetic solid phase microextraction based on ionic liquid-coated and cyclodextrin-functionalized magnetic core dendrimer nanocomposites for the determination of pyrethroids in juice samples.