1. Composites of polyamides and nanoparticles for dispersive micro-solid phase extraction
R. Lucena
Analytical Chemistry Department,
University of Córdoba, Spain

2. Combining polyamides and MNPs
Starting point
Combining polyamides and MNPs
Initial synthesis
Application
Nanocomposites in
food analysis
Versatility of polyamides
Selecting the monomers
Polyamides and SiO2 NPs
Effect on superficial area
Conclusions and further research

3. Starting point Potential of polymers, nanoparticles and their combination
E.M. Reyes- Gallardo, R. Lucena, S. Cárdenas and M. Valcárcel. Bioanalysis (2015) 7, 1723–1730

4. Nanometric size Micrometric size
Starting point Methods for the synthesis of composites
Core shell
NPs on the Polymer surface
Polymer
MNPs
Polymer
Nanometric size
Micrometric size
E.M. Reyes- Gallardo, R. Lucena, S. Cárdenas, M. Valcárcel.
J. Chromatogr. A, 1271, 2013, 50– 55.
M.C. Alcudia-León, R Lucena, S Cárdenas, M. Valcárcel
J. Chromatogr. A, 1455, 2016, 57-64

5. M.C. Alcudia-León, R Lucena, S Cárdenas, M. Valcárcel
Starting point Methods for the synthesis of composites
Core shell
Polymer
MNPs
Polymer
Nanometric size
M.C. Alcudia-León, R Lucena, S Cárdenas, M. Valcárcel
J. Chromatogr. A, 1455, 2016, 57-64

6. Nanometric size Micrometric size
Starting point Methods for the synthesis of composites
NPs on the Polymer surface
Polymer
MNPs
Polymer
Nanometric size
Micrometric size
E.M. Reyes- Gallardo, R. Lucena, S. Cárdenas, M. Valcárcel.
J. Chromatogr. A, 1271, 2013, 50– 55.

7. Naked polymeric fibers
Starting point Methods for the synthesis of composites
Electrospinning
Naked polymeric fibers
Composite

8. Combining polyamides and MNPs
Non-polar hydrocarbon backbone
Polyamide
MNPs
Polar amide group
FeCl2
FeCl3
MNPs
@SiO2
NH3
TEOS
H2O
Nylon 6
In formic acid
MNPs-nylon 6 omposite
Key factor: Switchable solubility of polyamides formic acid/water

9. Naked polymer Composite
Combining polyamides and MNPs
SEM micrographs
Naked polymer
Composite

10. Magnetic measurements
Combining polyamides and MNPs
ATR-IR
Magnetic measurements

11. Evaluation of the extraction performance
Combining polyamides and MNPs
Evaluation of the extraction performance
Dispersive micro-solid phase extraction procedure
Selected PAHs in water
HPLC-UV

12. Absolute extraction recovery 7.58%
Application Nanocomposite in food analysis
· Complex matrix
· Effect of precipitation on BPA recovery
· Extraction procedure in two steps
Protein clot—fat-BPA
Absolute extraction recovery 7.58%

13. Atenolol Propranolol Terephthalic acid
Versatility Selecting the monomers
Atenolol
Propranolol
Terephthalic acid

14. LODs in the range of 0.1-0.15 g/L Precision better than 9.6%
Versatility Selecting the monomers
LODs in the range of g/L
Precision better than 9.6%
Relative recoveries %

15. Synthesis Stages Composite SiO2-polyamides Effect on superficial area
Water
Filtration
Nylon-6 and SiO2 NPs in formic acid
Washing
Drying
Continuous magnetic stirring
Composite

16. S ≈ 17 m2/g S ≈ 87 m2/g SiO2-polyamides Effect on superficial area
The synthetic procedure increases de superficial area of the materials
S ≈ 17 m2/g
Pure nylon after synthetic procedure
S ≈ 87 m2/g
Nylon precursor
Synthesized composite

17. TEM micrographs SiO2-polyamides Effect on superficial area Silica NPs
Composite
Silica NPs

18. Extraction performance
SiO2-polyamides Effect on superficial area
Extraction performance
Type of solid
% of Nylon-6
% of Silica NPs A
100 B 75 25 C 50 D
E1  Estrone
E2  β-estradiol
E3  Estriol
Endogenous estrogens

19. Synergic combination of the polymer and NPs domains
Easy and cheap synthesis
Versatile
The interaction of some analytes with the composites is too intense
Manual synthesis
Extend the procedure to other polymer/NPs composition
Automate the syntheis
Evaluate other elution steps

20. Composites of polyamides and nanoparticles for dispersive micro-solid phase extraction
R. Lucena
Analytical Chemistry Department,
University of Córdoba, Spain