Search results for "010401 analytical chemistry"
showing 10 items of 1284 documents
Isolation of human milk whey proteins by solid phase extraction with a polymeric material modified with gold nanoparticles
2017
Abstract This work describes a method for the isolation of human milk whey proteins by solid-phase extraction (SPE) with a polymeric material modified with gold nanoparticles. Human serum albumin, α-lactalbumin, lactoferrin and lysozyme were selected as target proteins to establish the performance of SPE support. Several experimental variables (pH and ionic strength) that affect the SPE protocol were investigated to achieve the maximum extraction efficiency. Under optimal conditions, the SPE sorbent gave excellent recoveries, and offered a high permeability and reusability (> 20 times). The feasibility of this methodology was successfully demonstrated by isolating the target proteins in a m…
Poly(ethylene glycol) diacrylate-based solid-phase extraction for determination of sulfonamides in meat samples
2020
Abstract In this work, a sorbent based on poly(ethylene glycol) diacrylate (PEGDA) polymer has been synthesized for solid-phase extraction (SPE) of sulfonamides (sulfaguanidine, sulfadiazine, sulfathiazole, sulfapyridine, sulfamethazine, sulfamonomethoxine, sulfamethoxazole, sulfisoxazole) from different meat matrices, which were subsequently determined by HPLC-DAD. Several extraction parameters such as loading and elution solvents as well as other variables (loading capacity, breakthrough volume and reusability) influencing on the analytical performance of the sorbent were optimized. Under the optimal conditions, the developed method was successfully applied to determine the eight sulfonam…
Methylone determination in oral fluid using microextraction by packed sorbent coupled to ion mobility spectrometry
2020
Abstract A methodology based on microextraction by packed sorbent (MEPS) followed by ion mobility spectrometry (IMS) has been developed for the simple and automated determination of methylone in oral fluids. MEPS was carried out using a 100 µL eVol® XR hand-held automated analytical syringe filled with octadecyl silica sorbent. The effect of main experimental parameters of MEPS such as sample pH and ionic strength, number of aspirating/dispensing cycles, and elution solvent was studied to obtain a quantitative extraction of methylone. Oral fluid samples were spiked with methylone at different concentration levels from 50 to 400 µg L−1 and analyzed by the proposed MEPS-IMS procedure, giving …
Pesticide analysis in coffee leaves using a quick, easy, cheap, effective, rugged and safe approach and liquid chromatography tandem mass spectrometr…
2017
An analytical method using a quick, easy, cheap, effective, rugged and safe (QuEChERS) procedure for multi-residue determination of 52 pesticides in coffee leaf extractshas been developed and validated according to SANTE/11945/2015 guidelines. Different sorbent combinations for dispersive solid phase extraction (d-SPE) clean-up as well as dispersive liquid-liquid microextraction (DLLME) were tested. The relative standard deviations (RSDs) for the recovery of 87-94% of pesticides added to coffee leaf extracts,was ≤20% for samples spiked at concentrations up to 50ng*g-1 depending on the clean-up procedures. However, samples spiked with a 100ng*g-1 pesticide mixture gave RSDs>20% for most pest…
Reduced graphene oxide-based magnetic composite for trace determination of polycyclic aromatic hydrocarbons in cosmetics by stir bar sorptive dispers…
2020
This work describes a sensitive and rapid analytical method for trace determination of polycyclic aromatic hydrocarbons (PAHs) in cosmetic samples. The proposed method is based on stir bar sorptive-dispersive microextraction (SBSDME). A magnetic composite made of CoFe2O4 magnetic nanoparticles embedded into reduced graphene oxide sheets is used as sorbent phase. After the extraction, the target analytes are desorbed in toluene and then analyzed by gas chromatography-mass spectrometry (GC-MS). The main parameters involved in the extraction procedure (i.e., composite amount, extraction time and desorption time) were evaluated and optimized to provide the best extraction efficiency. The method…
Selection of sampling adsorbents and optimisation and validation of a GC-MS/MS method for airborne pesticides
2017
ABSTRACTA methodology for the sampling and determination of airborne pesticides has been developed. The trapping efficiency of three adsorbents, namely XAD-2,XAD-4 and a sandwich sorbent (PUF-XAD2-PUF), was tested for 34 pesticides and the latter was selected because it presented the highest retention capacity without breakthrough. Pesticides were determined by gas chromatography coupled to an ion trap mass spectrometer in tandem. The method showed recoveries ranging from 70% to 120% with limits of quantification in the range of 16.1–322.6 pg m−3 when 155 m3 were sampled. This analytical strategy was applied to 10 indoor air samples collected in dwellings from the Valencian Region. Six pest…
Modified magnetic-based solvent-assisted dispersive solid-phase extraction: application to the determination of cortisol and cortisone in human saliv…
2021
A modification of magnetic-based solvent-assisted dispersive solid-phase extraction (M-SA-DSPE) has been employed for the determination of the biomarkers cortisol and cortisone in saliva samples. M-SA-DSPE is based on the dispersion of the sorbent material by using a disperser solvent like in dispersive solid phase extraction (SA-DSPE) but a magnetic sorbent is used like in magnetic dispersive solid-phase extraction (M-DSPE). Thus, the magnetic sorbent containing the target analytes is retrieved using an external magnet like in M-DSPE. Finally, the analytes are desorbed into a small volume of organic solvent for the subsequent chromatographic analysis. To this regard, a M-SA-DSPE-based meth…
Sample preparation strategies for the determination of psychoactive substances in biological fluids
2020
This review focuses on the existing analytical procedures for the determination of new psychoactive substances (NPS) in biological fluids by chromatographic methods. Direct analysis of samples is scarcely employed and most proposed methodologies include a sample pre-treatment in order to remove matrix interferents and, in some cases, pre-concentrate extracts. Current extraction methods for NPS determination in plasma/serum, urine, and oral fluids have been widely discussed, such as liquid-liquid, solid-phase, and micro extraction approaches, highlighting the advantages and drawbacks of the proposed extraction methodologies. Regarding microextraction approaches, techniques like microextracti…
Dispersive micro-solid phase extraction
2019
Abstract Dispersive micro-solid phase extraction (D-μSPE) has gained special attention in the sample preparation process due to its simplicity, speed and efficiency. Different dispersion approaches have been used within this technique to allow a close contact between the sorbent and the donor sample solution during the entrapping step, but also between the sorbent and the solvent in the elution step. This dispersion favors the kinetics of both sorption and elution and therefore increases the efficiency of the overall extraction procedure. This technique boasts of high versatility owing to the great variety of solids available, covering a high range of chemical functionalities. This article …
Solid-phase extraction based on ground methacrylate monolith modified with gold nanoparticles for isolation of proteins
2015
In this study, a novel polymeric material functionalized with gold nanoparticles (AuNPs) was prepared as solid-phase extraction (SPE) sorbent for isolation of proteins. The sorbent was synthesized from a powdered poly(glycidyl-co-ethylene dimethacrylate) monolith, and modified with ammonia, followed by immobilization of AuNPs on the pore surface of the material. To evaluate the performance of this SPE support, proteins were selected as test solutes, being the extraction conditions and other parameters (loading capacity and regenerative ability of sorbent) established. The results indicated that this sorbent could be employed to selectively capture proteins according to their pI, on the basi…