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In-tube stir bar sorptive extraction based on 3-aminopropyl triethoxysilane surface-modified Ce-doped ZnAl layered double hydroxide thin film for determination of nonsteroidal anti-inflammatory drugs in saliva samples

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Abstract

A thin-film based on 3-aminopropyl triethoxysilane surface-modified Ce-doped zinc–aluminum layered double hydroxide was synthesized on the inner surface of an aluminum tube. It has been applied to in-tube stir bar sorptive extraction of nonsteroidal anti-inflammatory drugs in saliva samples followed by high-performance liquid chromatography. The sorbent was characterized by scanning electron microscopy, X-ray diffraction, Fourier-transform infrared spectroscopy, energy-dispersive X-ray spectroscopy, and elemental mapping. The extraction parameters including sample pH (4.2), extraction time (10 min), stirring speed (800 rpm), type of eluent (acidified tetrahydrofuran), eluent volume (100 μL), and desorption time (6 min) were thoroughly optimized. Under the optimum conditions, limits of detection were found to be less than 5.0 ng mL−1. Calibration plots were linear within the range 10–1000 ng mL−1 (R2 > 0.9982). Absolute recoveries were calculated in the range 63.5 to 72.4%. The repeatability (intra- and inter-day precision) and reproducibility (tube-to-tube precision) at concentrations of 50, 250, and 500 ng mL−1 were less than 7.6% and 9.4%, respectively. The method accuracy based on the relative error was calculated at these concentrations and ranged from − 4.9 to − 9.3% for intra-day relative error (%) and − 6.8 to − 11% for inter-day relative error (%). Finally, the method applicability was examined for the determination of nonsteroidal anti-inflammatory drugs in saliva samples, and good relative recoveries were obtained within the range 86.5 to 95.2%. As a result, the introduced method can be applied as a suitable alternative to measuring nonsteroidal anti-inflammatory drugs in biological fluids.

A surface-modified Ce-doped ZnAl LDH thin film was synthesized on the inner surface of an Al tube and applied for in-tube stir bar sorptive extraction of NSAIDs in saliva.

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Acknowledgments

The authors gratefully acknowledge the financial support provided by K.N. Toosi University of Technology (Tehran, Iran).

Author contribution statement

M.T.M.: conceptualization, methodology, validation, formal analysis, writing—original draft, visualization. S.S.: conceptualization, methodology, validation, software, resources, writing—review and editing, visualization, supervision, project administration. Y.R.: methodology, formal analysis, investigation. M.M.: formal analysis, writing—review and editing, validation. M.S.: methodology, investigation, resources.

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Authors and Affiliations

  1. Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, P.O. Box 16315-1618, Tehran, Iran

    Mahsa Torabi Mirzaee, Shahram Seidi, Yasaman Razeghi & Mahshid Manouchehri

  2. Analytical Chemistry Research Laboratory, Mobin Shimi Azma Company, Tehran, Iran

    Maryam Shanehsaz

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  1. Mahsa Torabi Mirzaee
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Correspondence to Shahram Seidi.

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All procedures in this study involving human participants were in accordance with the 1964 Helsinki Declaration and its later amendments or comparable ethical standards and performed with permission from the Educational and Research Committee (K. N. Toosi University of Technology) under the direct supervision of the Local Medical Clinic of the university (Approval Number 150796-L/28754).

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Mirzaee, M.T., Seidi, S., Razeghi, Y. et al. In-tube stir bar sorptive extraction based on 3-aminopropyl triethoxysilane surface-modified Ce-doped ZnAl layered double hydroxide thin film for determination of nonsteroidal anti-inflammatory drugs in saliva samples. Microchim Acta 187, 528 (2020). https://doi.org/10.1007/s00604-020-04489-z

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