Development, Characterization, and Applications of Universal Fabric Phase Sorptive Extraction Membrane for the Monitoring of Pollutants in Environmental Water and Food Samples

Authors

Basit Opeyemi Olayanju, Florida International UniversityFollow

Document Type

Dissertation

Degree

Doctor of Philosophy (PhD)

Major/Program

Chemistry

First Advisor's Name

Kenneth G. Furton

First Advisor's Committee Title

Committee chair

Second Advisor's Name

Abuzar Kabir

Second Advisor's Committee Title

Committee member

Third Advisor's Name

Anthony Decaprio

Third Advisor's Committee Title

Committee member

Fourth Advisor's Name

Golam Kibria

Fourth Advisor's Committee Title

Committee member

Fifth Advisor's Name

Christopher Dares

Fifth Advisor's Committee Title

Committee member

Keywords

Universal fabric phase sorptive extraction, sample preparation, sorbent, high performance liquid chromatograph-ultraviolet detector, environmental sample analysis, food sample analysis, analytical workflow, phthalates, endocrine disrupting chemicals, green analytical chemistry

Date of Defense

6-26-2023

Abstract

Sample preparation is an inevitable step involved in the analytical workflow and in fact, it consumes 60-80 percent of the total analysis time. In this study, a novel sorbent material considered to be ‘universal’ due to its ability to establish different intermolecular and interionic interactions such as hydrogen bond, π-π interaction, cationic exchange, anionic exchange, hydrophobic and hydrophilic interactions with the target compounds was coated on cellulose fabric substrate via sol-gel coating technology. The sorbent was characterized using SEM and FTIR to obtain the surface morphology information and functional groups of the constituting materials as well as the final product. Thereafter, the adsorption capability of the three formulations of the fabricated novel material (F3, F4 and F5) was conducted with ten test compounds of environmental concerns with varying polarity (log Kow values between 0.28 for furfuryl alcohol and 5.07 for diethylstilbestrol) using HPLC-UV in isocratic mode. The adsorption capability test indicated that F3 fortified with ix methyltrimethoxysilane (MTMS) (69.5%), 2-phenylethyl TMS (10%), methacryloxypropyl TMS (10%), mercaptopropyl TMS (5%), N-Trimethoxysilyl propyl N,N,N-Trimethylammonium chloride (5%), CH2Cl2, CH3OH in the ratio (7.00x10- 4 :1:0.14:0.14:0.5:0.06:5.6:8.88:4.83) demonstrated the best adsorption characteristics for these analytes and hence chosen for subsequent analytical applications for the monitoring of endocrine disrupting chemicals and phthalates in environmental water and milk sample. Linearity was recorded between 50-1000 ng/ml for dimethyl phthalate, 1-10000 ng/mL for di-n-heptyl phthalate, 1-5000 ng/mL for di-n-heptyl phthalate, 10-5000 ng/mL for di-n-ethylhexyl phthalate, 100-7500 ng/mL di-n-octyl phthalate, and 1-1000 ng/ml for others. The validated method was then applied for the assessment of phthalates in environmental water samples, bottled water, and juices. Secondly, we deployed the universal fabric phase sorptive extraction membrane in tandem with high performance liquid chromatograph equipped with ultraviolet detector for the analysis of ten (10) endocrine disruptors. Calibration curves were observed between 25 ppb to 2000 ppb for all compounds except cortisone in the range 25 ppb to 1000 ppb which gave R² value above 0.9940 in all cases. The validated method was deployed for the analysis of environmental water and whole milk samples with estradiol showing the highest concentrations among the studied compound.

Identifier

FIDC011165

ORCID

0000-0002-8473-3935

Previously Published In

• Câmara, José S., Rosa Perestrelo, Basit Olayanju, Cristina V. Berenguer, Abuzar Kabir, and Jorge A. M. Pereira. 2022. “Overview of Different Modes and Applications of Liquid Phase-Based Microextraction Techniques” Processes 10, no. 7: 1347. https://doi.org/10.3390/pr10071347. Citations: 2

• Câmara JS, Perestrelo R, Berenguer CV, Andrade CFP, Gomes TM, Olayanju B, Kabir A, M R Rocha C, Teixeira JA, Pereira JAM. Green Extraction Techniques as Advanced Sample Preparation Approaches in Biological, Food, and Environmental Matrices: A Review. Molecules. 2022 May 6;27(9):2953. doi: 10.3390/molecules27092953. PMID: 35566315; PMCID: PMC9101692. Citations: 35

Recommended Citation

Olayanju, Basit Opeyemi, "Development, Characterization, and Applications of Universal Fabric Phase Sorptive Extraction Membrane for the Monitoring of Pollutants in Environmental Water and Food Samples" (2023). FIU Electronic Theses and Dissertations. 5404.
https://digitalcommons.fiu.edu/etd/5404