Simple and selective extraction of quercetin with microextraction in packed syringe method using modified glass powder by a molecularly imprinted polymer followed by spectrophotometric determination.

A new sample preparation method based on microextraction in packed syringe was developed for preconcentration of quercetin prior to its spectrophotometric determination. Molecularly imprinted polymers as packing material was used for higher extraction efficiency. First, glass powder as support material because of low cost and available substrate was modified, and then molecularly imprinted polymers were synthesized by the sol-gel method using 3-aminopropyltriethoxysilane as a functional monomer and tetraethyl orthosilicate as cross-linker agent. The combination of a molecularly imprinted polymers and microextraction in packed syringe increased the selectivity and sensitivity. The surface morphology and functionality of the prepared molecularly imprinted polymers was characterized using Fourier-transform infrared spectroscopy, Field emission scanning electron microscopy, energy dispersive X-ray spectroscopy, and thermogravimetric analysis. Different influencing parameters on extraction efficiency such as effect of the number of sample sorption/desorption cycles, type and volume of desorption solvent, pH of the sample solution, and molecularly imprinted polymers amounts were optimized. Under the optimum condition, the proposed method displayed a linear range from 0.01 to 5 µg mL-1 and limit of detection 3.68 ng mL-1 . Relative standard deviation for three replicate determination of 1 µg mL-1 quercetin was 2.1 %. The proposed method was applied successfully for the selective extraction of quercetin from tea and coffee samples.

Preconcentration of Pb(II) by Magnetic Metal-Organic Frameworks and Analysis Using Graphite Furnace Atomic Absorption Spectroscopy.

In this study, a magnetic metal-organic framework (MOF) was synthesized based on magnetic Fe3O4, Cu(II), and benzene-1,3,5-tricarboxylic acid (Cu-BTC) as a sorbent for solid phase extraction (SPE) of trace amounts of Pb(II) in water and lettuce samples. Pb(II) ion was adsorbed on the magnetic MOF and easily separated by a magnet; therefore, no filtration or centrifugation was necessary. The analyte ions were eluted by HCl 0.5 mol·L-1 and analyzed via graphite furnace atomic absorption spectroscopy. The prepared sorbent was characterized by scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), and Fourier transform-infrared (FT-IR) spectroscopy. Under optimal experimental conditions, the method had a linear range of 0.1-50 µg·L-1. The limits of detection and quantitation for lead were found to be 0.026 and 0.08 µg·L-1, respectively. The results showed that the prepared sorbent has high selectivity for Pb2+ even in the presence of other interfering metal ions.

Indirect determination of mercury(II) by using magnetic nanoparticles, CdS quantum dots and mercury(II)-binding aptamers, and quantitation of released CdS by graphite furnace AAS.

This work describes an aptamer based method for highly sensitive determination of Hg(II). A Hg(II)-binding ssDNA aptamer was linked to silica-coated magnetic nanoparticles (magNPs). Then, a conjugate composed of graphene and CdS quantum dots (Gr-CdS) was linked to the complementary ssDNA. On mixing the two components, a duplex of type magNP-dsNNA-Gr/CdS is generated. If Hg(II) is added, it wills capturing the aptamer, and this leads to the release of Gr/CdS because of the formation of a stable thymine-Hg2+-thymine link. External magnetic force is used to remove the remaining complex. The released graphene-CdS is decomposed by HNO3 and injected into a graphite furnace AAS. The detectable amount of Cd is proportional to the concentration of Hg(II) in the sample. Under the optimal conditions, the method has a linear response in the 2.50 aM to 0.25 nM Hg(II) concentration range, and the detection limit is as low as 7.6 aM (at S/N = 3). It has high selectivity for Hg(II) over other metal ions. Graphical abstract.