PMID- 33743514 OWN - NLM STAT- MEDLINE DCOM- 20210628 LR - 20210628 IS - 1873-376X (Electronic) IS - 1570-0232 (Linking) VI - 1171 DP - 2021 May 1 TI - Ultrasound-assisted solid phase microextraction-HPLC method based on Fe(3)O(4)@SiO(2)-NH(2)-molecularly imprinted polymer magnetic nano-sorbent for rapid and efficient extraction of harmaline from Peganum harmala extract. PG - 122640 LID - S1570-0232(21)00120-3 [pii] LID - 10.1016/j.jchromb.2021.122640 [doi] AB - In the present study, a magnetic molecularly imprinted polymer (MMIP) was synthesized for the extraction of harmaline from Peganum harmala by dispersive solid-phase microextraction (DSPME). The MMIP for selective and intelligent extraction of harmaline with excellent functionality and high selectivity was synthesized using the sol-gel method with functionalized superparamagnetic core-shell nanoparticles, ethylene glycol dimethacrylate (EDMA) as a cross-linker, methacrylic acid (MAA) as a functional monomer, and 2,2-azobisisobutyronitrile (AIBN) as a porogen. To study the properties and morphology of the coated polymer, FT-IR spectroscopy, FESEM, TEM images, and VSM were used. The DSPME-HPLC-UV equipment was used to quantify and analyze the data obtained from harmaline extraction. In this research, the efficiency of the synthesized polymer in harmaline extraction was modeled and optimized using the response surface methodology based on central composite design (RSM-CCD). In addition, for modeling the isotherm of harmaline sorption by the MMIP, Langmuir and Freundlich isotherm equations were used. The obtained results showed that the extraction of harmaline with the MMIP was well described with Freundlich isotherm. The results of the validation of the method showed that the measurement of harmaline in the concentration range of 1.0-4000 ng mL(-1) followed a linear relationship (R(2) = 9986.0). Moreover, the accuracy or repeatability index (% RSD) was determined to be < 10, and the LOQ and LOD values were 0.526 and 0.158 ng mL(-1), respectively. The results of this study showed that the DSPME technique by using the synthesized MMIP as an effective sorbent with high efficiency and capacity could be utilized for pre-concentration and extraction of harmaline from real and complex samples. CI - Copyright (c) 2021 Elsevier B.V. All rights reserved. FAU - Sadegh, Negar AU - Sadegh N AD - Department of Chemistry, Faculty of Sciences, Shahrekord University, P.O. Box 115, Shahrekord, Iran. FAU - Asfaram, Arash AU - Asfaram A AD - Medicinal Plants Research Center, Yasuj University of Medical Sciences, Yasuj, Iran. Electronic address: arash.asfaram@yums.ac.ir. FAU - Javadian, Hamedreza AU - Javadian H AD - Department of Chemical Engineering, ETSEIB, Universitat Politecnica de Catalunya, Diagonal 647, 08028 Barcelona, Spain. FAU - Haddadi, Hedayat AU - Haddadi H AD - Department of Chemistry, Faculty of Sciences, Shahrekord University, P.O. Box 115, Shahrekord, Iran. FAU - Sharifpour, Ebrahim AU - Sharifpour E AD - Social Determinants of Health Research Center, Yasuj University of Medical Sciences, Yasuj, Iran. LA - eng PT - Journal Article DEP - 20210309 PL - Netherlands TA - J Chromatogr B Analyt Technol Biomed Life Sci JT - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JID - 101139554 RN - 0 (Magnetite Nanoparticles) RN - 0 (Molecularly Imprinted Polymers) RN - 0 (Plant Extracts) RN - CN58I4TOET (Harmaline) SB - IM MH - Chromatography, High Pressure Liquid/*methods MH - *Harmaline/analysis/chemistry/isolation & purification MH - Limit of Detection MH - Linear Models MH - Magnetite Nanoparticles/*chemistry MH - Molecular Imprinting/methods MH - Molecularly Imprinted Polymers/*chemistry MH - Peganum/*chemistry MH - Plant Extracts/chemistry MH - Reproducibility of Results MH - Solid Phase Microextraction/methods MH - Sonication/methods OTO - NOTNLM OT - DSPME-HPLC-UV OT - Harmaline OT - Magnetic molecularly imprinted polymer (MMIP) OT - Solid-phase microextraction EDAT- 2021/03/21 06:00 MHDA- 2021/06/29 06:00 CRDT- 2021/03/20 20:20 PHST- 2021/01/24 00:00 [received] PHST- 2021/02/23 00:00 [revised] PHST- 2021/02/27 00:00 [accepted] PHST- 2021/03/21 06:00 [pubmed] PHST- 2021/06/29 06:00 [medline] PHST- 2021/03/20 20:20 [entrez] AID - S1570-0232(21)00120-3 [pii] AID - 10.1016/j.jchromb.2021.122640 [doi] PST - ppublish SO - J Chromatogr B Analyt Technol Biomed Life Sci. 2021 May 1;1171:122640. doi: 10.1016/j.jchromb.2021.122640. Epub 2021 Mar 9.