Ultrasound-assisted solid phase microextraction-HPLC method based on Fe3O4@SiO2-NH2-molecularly imprinted polymer magnetic nano-sorbent for rapid and efficient extraction of harmaline from Peganum harmala extract

Negar Sadegh; Arash Asfaram; Hamedreza Javadian; Hedayat Haddadi; Ebrahim Sharifpour

doi:10.1016/j.jchromb.2021.122640

Ultrasound-assisted solid phase microextraction-HPLC method based on Fe₃O₄@SiO₂-NH₂-molecularly imprinted polymer magnetic nano-sorbent for rapid and efficient extraction of harmaline from Peganum harmala extract

J Chromatogr B Analyt Technol Biomed Life Sci. 2021 May 1:1171:122640. doi: 10.1016/j.jchromb.2021.122640. Epub 2021 Mar 9.

Authors

Negar Sadegh¹, Arash Asfaram², Hamedreza Javadian³, Hedayat Haddadi¹, Ebrahim Sharifpour⁴

Affiliations

¹ Department of Chemistry, Faculty of Sciences, Shahrekord University, P.O. Box 115, Shahrekord, Iran.
² Medicinal Plants Research Center, Yasuj University of Medical Sciences, Yasuj, Iran. Electronic address: arash.asfaram@yums.ac.ir.
³ Department of Chemical Engineering, ETSEIB, Universitat Politècnica de Catalunya, Diagonal 647, 08028 Barcelona, Spain.
⁴ Social Determinants of Health Research Center, Yasuj University of Medical Sciences, Yasuj, Iran.

PMID: 33743514
DOI: 10.1016/j.jchromb.2021.122640

Abstract

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 (R² = 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.

Keywords: DSPME-HPLC-UV; Harmaline; Magnetic molecularly imprinted polymer (MMIP); Solid-phase microextraction.

MeSH terms

Chromatography, High Pressure Liquid / methods*
Harmaline* / analysis
Harmaline* / chemistry
Harmaline* / isolation & purification
Limit of Detection
Linear Models
Magnetite Nanoparticles / chemistry*
Molecular Imprinting / methods
Molecularly Imprinted Polymers / chemistry*
Peganum / chemistry*
Plant Extracts / chemistry
Reproducibility of Results
Solid Phase Microextraction / methods
Sonication / methods

Substances

Magnetite Nanoparticles
Molecularly Imprinted Polymers
Plant Extracts
Harmaline