Highly Selective Determination of Chrysoidine in Foods Through a Surface Molecularly Imprinted Sol–Gel Polymer Solid-Phase Extraction Coupled with HPLC

A highly selective determination method for chrysoidine, an industrial azoic dye banned in foods, was developed through a novel molecularly imprinted polymer (MIP) online solid-phase extraction coupled with high-performance liquid chromatography. The MIP was firstly synthesized by a surface molecular imprinting technique in combination with a sol–gel process and characterized by FT-IR and adsorption experiments. The MIP exhibited high selectivity and high adsorption capacity for chrysoidine and offered a fast kinetics for the adsorption and desorption of chrysoidine. A number of parameters, including the pH of loading solution, the sample loading flow rates, and eluting time of analyte, were carefully optimized to improve the extraction efficiency. Under the optimal experimental conditions, for a 50-mL sample solution, the enrichment factor was 279 and the detection limit (S/N?=?3) was 6 ng L^?1. The linear plots with r ²?>?0.99 were achieved over a range of 0.04–40 μg L^?1, and the peak area precision (relative standard deviation) for nine parallel determinations was below 6.32 %. This method was employed for quantitative determination of chrysoidine in oil bean curd, yellow croaker, and paprika with satisfactory recoveries (89.3–97.6 %).     

Solid-Phase Extraction of Florfenicol from Meat Samples by a Newly Synthesized Surface Molecularly Imprinted Sol–Gel Polymer

A new molecularly imprinted polymer (MIP) as a solid-phase sorbent for selective extraction of florfenicol (FF) was prepared by combination of the surface molecular imprinting technique with the sol–gel process. The FF-imprinted silica sorbent was prepared using FF as template, 3-aminopropyltriethoxysilane as functional monomer and tetraethoxysilicate as cross-linker on the silica gel support. The non-imprinted silica (NIP) was synthesized in the same way without addition of FF. The MIP was evaluated as a sorbent in column extraction approach for extraction of FF from aqueous solutions followed by spectrofluorometric determination. The influence of certain variables including the sample pH, the sample volume, the sample flow rate, the type of eluent, and its flow rate on the extraction efficiency of FF was assessed. The prepared FF-MIP silica sorbent showed higher adsorption capacity (64.9 mg g^?1) and significant selectivity than the corresponding NIP (11.5 mg g^?1). The FF-MIP-based solid phase extraction method was successfully applied to the separation and determination of FF from fish and chiken meat samples under the optimized extraction conditions.     

Ultrasound-Assisted Extraction Followed by Solid-Phase Extraction Followed by Dispersive Liquid–Liquid Microextraction for the Sensitive Determination of Diazinon and Chlorpyrifos in Rice

Selectivity of solid-phase extraction (SPE) was combined with the concentration power of dispersive liquid–liquid microextraction (DLLME) to obtain a sensitive, low solvent consumption method for high-performance liquid chromatography determination of diazinon and chlorpyrifos in rice. In this method, rice samples were extracted by ultrasound-assisted extraction followed by SPE. Then, the SPE eluent was used as a disperser solvent in the next dispersive liquid-liquid microextraction step for further purification and enrichment of diazinon and chlorpyrifos. Under the optimal conditions, the linear range was from 5.0 to 250 μg kg^?1 for diazinon and from 2.5 to 250 μg kg^?1 for chlorpyrifos. Limits of detection of diazinon and chlorpyrifos were 1.5 and 0.7 μg kg^?1, respectively. Limits of quantitation of diazinon and chlorpyrifos were 5.5 and 3.0 μg kg^?1, respectively. The precisions and recoveries also were investigated by spiking 10 μg kg^?1 concentration in rice. The recoveries obtained were over 90 % with relative standard deviation (RSD%) below 9.0 %. The new approach was utilized to successfully detect trace amounts of diazinon and chlorpyrifos in different Iranian rice samples.     

Modified QuEChERS Combination with Magnetic Solid-Phase Extraction for the Determination of 16 Preservatives by Gas Chromatography–Mass Spectrometry

In this paper, based on the mechanism of the quick, easy, cheap, effective, rugged and safe (QuEChERS) method, a novel graphene grafted silica-coated Fe₃O₄ (Fe₃O₄@SiO₂@G) was synthesized and applied as the efficient magnetic solid-phase extraction (MSPE) adsorbent for rapid cleanup of vegetable samples prior to analyzing 16 preservative residues by gas chromatography–mass spectrometry (GC-MS). The method, which took advantages of the novel nanoparticle adsorbent and an external magnetic field separation targets from samples, not only could avoid the time consuming of the traditional solid-phase extraction, but also could be developed for simultaneous determination of 16 preservative residues in vegetables. Various experimental parameters that could affect the extraction efficiencies have been investigated. Under the optimum conditions, 16 preservatives showed good linearity over the range of 0.02–2.00 mg/L and correlation coefficients (R ²) of 0.9946–0.9998. The limits of detections (LODs) were in the range of 0.21–11.50 μg/kg. The recoveries of 16 preservatives ranged from 78.3 to 116.7 %, and the relative standard deviations (RSDs) ranged from 1.4 to 11.9 %.     

Coating of Sol–Gel Film on Silver Nanodendrite as a Novel Solid-Phase Microextraction Fiber for Determination of Volatile Aldehydes in Edible Oils

In this work, a novel solid-phase microextraction fiber was fabricated by a new substrate applied for quantitative analysis of trace volatile aldehydes emitted during thermal oxidation of edible oils, analyzed by GC–MS. Ag nanodendrites as a porous substrate, spontaneously coated on a Cu wire, and polydimethylsiloxane/polyethylene glycol (PDMS/PEG) were deposited onto the substrate by sol–gel dip-coating. Parameters affecting the extraction efficiency, such as the substrate porosity, extraction time and temperature, and desorption time and temperature were investigated and optimized. The desorption temperature was chosen as 260 °C, and desorption time was set at 3 min. Results shows that extraction efficiency of sol–gel coating deposited on Ag nanodendrite substrate is meaningfully higher than that of deposited on bare Cu wire. Under the optimum conditions, the limits of detection (LODs) ranged between 0.5 to 0.2 μg/L. The relative standard deviations including repeatability (within fibers) and reproducibility (between fibers) varied between 7.5–11.2 and 9.3–16.2%, respectively.     

A Rapid Size-Exclusion Solid-Phase Extraction Step for Enhanced Sensitivity in Multi-Allergen Determination in Dark Chocolate and Biscuits by Liquid Chromatography–Tandem Mass Spectrometry

Enhanced sensitivity for the simultaneous determination of five nut allergens in biscuit and in dark chocolate complex matrices was obtained by introduction of a rapid size-exclusion solid-phase extraction-based step before liquid chromatography–electrospray ionization-tandem mass spectrometry (LC-ESI-MS²) analysis. A very fast and efficient separation (<12 min) of marker peptides with selected reaction monitoring detection was obtained. Limits of detection in the 0.1–1.3 mg nut/kg and 5–15 mg nut/kg ranges for biscuit and dark chocolate samples as well as high recoveries (84(±6)–106(±4)% for biscuits and 98(±5)–108(±6)% for dark chocolate) proved the excellent capabilities of the exploited sample treatment method combined with the LC-MS² analysis. Good precision in terms of intra- and inter-day repeatability was calculated, being always lower than 19 % (n?=?75). Linearity was demonstrated up to four and three orders of magnitude for biscuit and dark chocolate, respectively. Finally, the validated method was successfully applied to the investigation of hidden nut trace allergens in commercially available biscuits and chocolates of different brands aiming to ascertain possible discrepancies between allergen content and food allergen labelling.