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Hollow mesoporous structured molecularly imprinted polymer as adsorbent in pipette‐tip solid‐phase extraction for the determination of antiretrovirals from plasma of HIV‐infected patients

Simões, Nathália Soares, de Oliveira, Hanna Leijoto, da Silva, Ricky Cássio Santos, Teixeira, Leila Suleimara, Sales, Thaís Lorenna Souza, de Castro, Whocely Victor, de Paiva, Maria José Nunes, Sanches, Cristina, Borges, Keyller Bastos
Electrophoresis 2018 v.39 no.20 pp. 2581-2589
HIV infections, Human immunodeficiency virus, acetonitrile, adsorbents, antiretroviral agents, benzalkonium chloride, chemical species, electrophoresis, ethylene glycol, high performance liquid chromatography, lamivudine, monitoring, pH, patients, polymers, porous media, solid phase extraction, solvents, statistical analysis, surfactants, therapeutics
In this work a hollow mesoporous structured molecularly imprinted polymer was synthetized and used as adsorbent in pipette‐tip solid‐phase extraction for the determination of lamivudine (3TC), zidovudine (AZT) and efavirenz (EFZ) from plasma of human immunodeficiency virus (HIV) infected patients by high‐performance liquid chromatography (HPLC). All parameters that influence the recovery of the pipette tip based on hollow mesoporous molecularly imprinted polymer solid‐phase extraction (PT–HM–MIP–SPE) method were systematically studied and discussed in detail. The adsorbent material was prepared using methacrylic acid and 4‐vinylpyridine as functional monomers, ethylene glycol dimethacrylate as crosslinker, acetonitrile as solvent, 4,4′‐azobis(4‐cyanovaleric acid) as radical initiator, benzalkonium chloride as surfactant, 3TC, and AZT as templates. The simultaneous separation of 3TC, AZT and EFZ by HPLC‐UV was performed using a Gemini C18 Phenomenex® column (250 mm × 4.6 mm, 5 μm) and mobile phase consisting of acetonitrile: water pH 3.2 (68:32, v/v), flow rate of 1.0 mL/min and λ = 260 nm. The method was linear over the concentration range from 0.25 to 10 μg/mL for 3TC and EFZ, and 0.05 to 2.0 μg mL⁻¹ for AZT, with correlation coefficients larger than 0.99 for all analytes. Recovery ± relative standard deviations (RSDs %) were 41.99 ± 2.38%, 82.29 ± 1.63%, and 83.72 ± 7.52% for 3TC, AZT, and EFZ, respectively. The RSDs and relative errors (REs) were lower than 15% for intra and interday assays. The method has been successfully applied for monitoring HIV‐infected patients outside the therapeutic dosage.