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Sample preparation of complex matrices is commonly performed using either liquid-based or sorbent-based extraction techniques, which have been developed and utilized in numerous variations. Pipette-tip microextraction is a relatively recent technique that has proven to be an effective approach for sample preparation. Various materials have been utilized in this technique including monoliths, silica-based, paper-based, functionalized-inner wall pipette tips and nature-derived materials. However, some of these approaches assist in tip clogging, they still face the issue of prolonged extraction times. In this study, the commercially available Salivette® synthetic material is proposed as a cost-effective extraction sorbent using the pipette tip format. To evaluate the effectiveness of the proposed method, the determination of urinary memantine was chosen as a case study. The sorbent was cut into semicircles and incorporated into 1 mL pipette tip without frits. The proposed approach offers comparable/improved results relative to previous published pipette tip extraction techniques while it minimizes the number of aspirating/dispensing steps, thereby reducing analyst fatigue. The drug was derivatized prior its determination by liquid chromatography and fluorescence detection. Excellent linearity in the range of 5 - 500 ng/mL (r > 0.9920), adequate intra-day and inter-day precision (<14.7 %) and recoveries (ranged between 87.4-115.9 % in all cases) were observed. The limit of detection and the lower limit of quantitation were 1 and 5 ng/mL, respectively. A single washing step of undiluted urine appeared to be sufficient to eliminate the matrix effects. The reported research demonstrated that the biocompatible Salivette® sorbent can be successfully used in pipette tip microextraction. It is commercially available, eliminating the need for the synthesis and characterization of new materials. It requires small amounts of solvents per analysis, supporting the principles of Green Sample Preparation. To enhance sample throughput, a multichannel pipette could also be considered. The innovation and the green character of the analytical scheme were evaluated using the newly developed Violet Innovation Grade Index and AGREEprep tools.
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http://dx.doi.org/10.1016/j.chroma.2025.466316 | DOI Listing |
Anal Sci
September 2025
Key Laboratory of Poyang Lake Environment and Resource Utilization, Ministry of Education, School of Resources and Environment, Nanchang University, Nanchang, 330031, People's Republic of China.
The accurate detection of trace perfluoroalkyl acids (PFAAs) in drinking water remains challenging due to nonspecific adsorption losses during pretreatment. This study systematically evaluated the adsorption behaviors of 11 PFAAs across five filtration membranes and four solid-phase extraction (SPE) sorbents to establish an optimized analytical protocol. Results demonstrated that glass fiber (GL) filters minimized PFAAs retention (94.
View Article and Find Full Text PDFACS Omega
September 2025
Research Laboratory in bionanomaterials, LPbio, Department of Chemistry, Federal University of Viçosa, 36570-900 Viçosa, Minas Gerais, Brazil.
Herein, it is reported the synthesis of a niobium-based metal-organic framework (MOF), [Nb-(Bez-(COO))] , for the extraction of caffeine from surface waters. The material was synthesized and characterized by Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD), and Brunauer-Emmett-Teller (BET) analysis, which confirmed the coordination between the ligand (1,4-benzenodicarboxylic, (Bez-(COO))) and niobium (Nb) with a morphology composed of hexagonal rods, high crystallinity, and a surface area of 94.7 m g.
View Article and Find Full Text PDFAnal Chim Acta
November 2025
Department of Analytical Chemistry, Faculty of Chemistry, Alzahra University, Vanak, Tehran, Iran; Analytical and Bioanalytical Research Centre, Alzahra University, Vanak, Tehran, Iran. Electronic address:
Background: Determination of the estradiol hormone in urine is crucial for evaluating congenital adrenal hyperplasia, certain hormone-producing ovarian tumors, polycystic ovary syndrome, liver disease, pregnancy, and infertility. On the other hand, steroid hormones can have destructive effects on the environment, animals, and the endocrine system of humans. Consequently, accurately measuring this hormone's concentration in trace amounts is essential for environmental safety and human health.
View Article and Find Full Text PDFSci Rep
September 2025
Food and Drug Safety Research Center, Tabriz University of Medical Sciences, Tabriz, Iran.
An in-situ CO₂-assisted dispersive micro solid phase extraction was developed using a covalent organic framework synthesized from melamine and barbituric acid as a sorbent for the extraction of Cd(II) and Zn(II) ions from honey samples. The structural and morphological characteristics of the sorbent were evaluated using scanning electron microscopy, X-ray diffraction, and Fourier transform infrared spectrometry. The CO₂ generated by reacting tartaric acid and sodium hydrogen carbonate enabled rapid dispersion of the sorbent within the sample solution, ensuring optimal contact with the target ions.
View Article and Find Full Text PDFAnal Bioanal Chem
September 2025
Department of Analytical, Bioanalytical Sciences and Miniaturization (LSABM), Chemistry, Biology and Innovation (CBI), UMR 8231 ESPCI Paris - CNRS, ESPCI Paris, PSL University, 10 Rue Vauquelin, 75005, Paris, France.
The ratio between beta-amyloid (Aβ) peptides 40 and 42 is recognized as a biomarker for Alzheimer's disease, playing a significant role in early diagnosis and disease progression monitoring. Aβ peptides are present at trace levels in cerebrospinal fluid, therefore, developing a new selective extraction procedure is essential for isolating targeted biomarkers from the matrix interferents, ensuring accurate identification and quantification. In this study, a hybrid organic-silica monolith was synthesized in a 530 µm inner diameter-capillary and used for the covalent grafting of beta amyloid peptide aptamers.
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