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Steroid hormones are active substances that are necessary in the normal functioning of all physiological activities in the body, such as sexual characteristics, metabolism, and mood control. They are also widely used as exogenous chemicals in medical and pharmaceutical applications as treatments and at times growth promoters in animal farming. The vast application of steroid hormones has resulted in them being found in different matrices, such as food, environmental, and biological samples. The presence of hormones in such matrices means that they can easily come into contact with humans and animals as exogenous compounds, resulting in abnormal concentrations that can lead to endocrine disruption. This makes their determination in different matrices a vital part of pollutant management and control. Although advances in analytical instruments are constant, it has been determined that these instruments still require some sample preparation steps to be able to determine the occurrence of pollutants in the complex matrices in which they occur. Advances are still being made in sample preparation to ensure easier, selective, and sensitive analysis of complex matrices. Molecularly imprinted polymers (MIPs) have been termed as advanced solid-phase (SPE) materials for the selective extraction and preconcentration of hormones in complex matrices. This review explores the preparation and application of MIPs for the determination of steroid hormones in different sample types.

Neonicotinoid insecticides have raised a lot of societal concerns due to their environmental ubiquity and unique mode of action. Therefore, it is of great research interest to monitor their occurrence in the environmental waters. However, these compounds exist at low concentrations that is below instrument detection limits. This study reports the applicability of magnetic poly (3 aminobenzoic acid)-based activated carbon (Fe3O4@PABA/AC) composite as an adsorbent in dispersive magnetic solid-phase microextraction (d-MSPME) of neonicotinoid insecticides from wastewater and river water samples. The as-synthesized adsorbent was characterized and confirmed by Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, Brunauer–Emmett–Teller and X-ray diffraction spectroscopy. The analytes of interest were detected and quantified by high-performance liquid chromatography coupled with diode array detector (HPLC–DAD). The parameters affecting the extraction and preconcentration processes, such as pH, extraction time, mass of adsorbent, desorption time and eluent volume, were optimized using fractional factorial design and central composite design. Under optimum conditions, the limits of detection and quantification were in the ranges of 0.41–0.82 µg L−1 and 1.4–2.7 µg L−1, respectively. The linearity ranged from 1.4–700 µg L−1 with correlation of determination (R2) values varied between 0.9933 and 0.9987. The intra-day and inter-day precisions were 0.35–0.75% and 1.7–5.5%, respectively. The spike recovery experiments were conducted to evaluate the accuracy of the d-MSPME analytical method in real samples, and the percentage recoveries ranged from 86.7 to 99.2%. Therefore, this method shows great potential applicability in preconcentrating the pollutants from the environment.

Neonicotinoid insecticides are widely used to kill and prevent unwanted insects from attacking growing crops. Extensive use of insecticides in various compartments of the environment has led to adverse effect on the health of living organisms. Several analytical methodologies have been reported for extraction and quantification of neonicotinoid insecticides in various matrices. The analytical detection techniques range from traditional to modern or state of the art quantification methods. The traditional analytical techniques include gas chromatography and high-performance liquid chromatography. These methods require extensive sample pretreatment before identification, separation, and quantification of target analytes. Advanced detection techniques refer to the sensor technologies based on optical, biorecognition, molecular imprinted polymers chemical, and piezoelectric. In this review, a summary and explanation of the various traditional analytical and advanced methodologies for extraction, separation, detection, and quantification of neonicotinoid insecticides residue in water samples have been discussed.

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In this study, a magnetic porphyrin-based porous organic polymer (MP-POP) nanocomposite was successfully synthesized according previous studies and applied as an adsorbent for simultaneous extraction and preconcentration of four neonicotinoid insecticides from surface river water. The MP-POP was characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy/energy dispersive x-ray spectroscopy (SEM/EDS), N 2-adsorption/desorption analysis, Fourier Transform infrared spectroscopy (FTIR). The neonicotinoid insecticides were quantified using high performance chromatography coupled with diode array detector (HPLC-DAD). The MP-POP shown to have a high surface area, highly porous structure and strong affinity toward the investigated analytes. The adsorption capacities were 99.0, 85.5, 90.0, and 79.4 mg g −1 for acetamiprid, clothiandin, thiacloprid and imidacloprid, respectively. The influential parameters affecting the magmatic µ-solid phase extraction (M-µ-SPE) procedure were investigated using fractional factorial design and surface response methodology (RSM). Under optimum conditions, the method exhibited relatively low limit of detection in the range of 1.3-3.2 ng L −1 , limit of quantification in the range of 4.3-11 ng L −1 and wide linearity (up to 600 µg L −1). The intraday and interday precision, expressed as the relative standard deviation (RSD) were <5%. The percentage recoveries for the four target analytes ranged from 91 to 99.3% for the spiked river water samples. The method was applied for determination of neonicotinoids in river water samples and concentrations ranged from 0 to 190 ng L −1 .

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