Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Task 2.4 Provision of the novel antibacterial NPs

Partners: UPC, SYN, CNR, BIU, CENTI

Antibacterial NPs

Inorganic NPs

ZnxCu1-xO

Ga@C-dots

Si/TiO2,Ag@HEC, TiO2@SiO2, CuO-ASC

Polymer NPs

Polypyrrole (PPy)

Biologicals

function-spacer-lipid constructs (FSLs)

antimicrobial enzymes

R2R US 2D (both sides) coating

Batch US 3D coating

R2R spray US 2D (one side) coating

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Task 2.4 Provision of the novel antibacterial NPs

Antimicrobial textiles

Active agents

Inorganic NPs: Si/TiO2, Zn 0.89 Cu 0.11O, ZnxCu1-xO, and Ga@C-dots Polymers - PPy

Coating

process

Single step processes

Both sides R2R sonochemical coating: one step in situ NPs production and coating, or “throwing stones” coating of NPs with high durability without any additional pre- or post-

treatment One side R2R spray coating: spraying of customised NP formulations

Anti-microbial and anti-biofilm water treatment membranes

Active

agents

Inorganic or PPy NPs (0.5%w/w)

Coating

process The two R2R continuous processes

Antimicrobial, anti-biofilm and biocompatible medical devices

Active

agents

Inorganic NPs (~0.4% w/w)

Organic NPs (0.5-1% w/w) PPy, FSLs and biologicals, e.g. antimicrobial/antibiofilm enzymes

Coating

process

Sonochemical batch process: One step in situ NPs production and coating, or

“throwing stones” embedding of ready-to-use NPs

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Sol-gel technology for synthesis and engineering of antibacterial NPs

Ag@HEC, TiO2@SiO2, CuO-ASC

Customised nanosols for spray and US R2R and batch coating

Inorganic NPs (BIU, CNR-ISTEC)

Sonochemical technology for synthesis and coating of antibacterial NPs

MeO and doped MeO (ZnO, CuO, Zn-CuO), Ga@C-dots

Protocols for in-situ NP synthesis and US coating

(batch and R2R)

Customised NPs for R2R and batch coating

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Inorganic NPs (BIU)

Novel composite ZnxCu1-xO NPs kill bacteria

10,000-100,000 times better than CuO or ZnO

NPs alone

Doped MeO - hydrolysis of metal acetates in

9:1 ethanol/water solution under US. molar

ratio between copper acetate and zinc acetate

is 3:1

Sonochemical technology

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Ga@C-dots - sonication of solution of Ga in PEG 400 yields NPs with narrow size

distribution (7±2 nm) and crystalline structure

Optimisation will include changing the initial concentration of Ga and various organic

solvents will be used

Inorganic NPs (BIU)

Sonochemical technology

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Ag@HEC - antimicrobial hybrid NPs patented by CNR

AgNO3

HEC

+ NaOH = Ag@HEC

- Gel with tunable viscosityfrom gel to liquid

Precursor

Catalyst

Higher antimicrobial activity and lower cytotoxicity compared to

commercial AgNPs

HEC improves the

integration with

cellulosic substrates

IC50 values A431

Calcein Resazurin

AgRef 21.87 9.33

AgHEC 45.7 21.87

AgRef

AgHEC

073E. Coli Strain CFT

Easy transferable synthesis to the pilot lines (spray and US coating)

AgNPs nucleate at RT into the hydroxyethylcellulose matrix

Inorganic NPs (CNR-ISTEC) Sol-gel technology

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Ratio TiO2:SiO2 1:3

Bright particles : TiO2

Grey matrix: SiO2

TiO2@SiO2 nanosol by a safer by design strategy

Performance evaluation: NOx abatement

0

100

200

300

400

500

600

0 50 100 150

Co

nce

ntr

atio

n N

O (

pp

bv)

Time (min)

TiO2_6

TiO2_37_Sil

TiO2_18_SilSamples with silica ROS SiO2

Key Risk properties: ROS production

•Enhanced photocatalytic activity of TiO2

•Reduced production of ROS

•Potentiated antibacterial efficiency of TiO2

Inorganic NPs (CNR-ISTEC) Sol-gel technology

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Preparation

STOCK WATER

suspensions

(10g /L)

Sodium Ascorbate

Maximising

nanofraction and

adhesion of coating

agents

by WET BALL MILLING

Introduction of modifiers

by self-assembling

CuOH2(+)

CuO

CuO@ASC nanosol by a safer by design strategy

Material LC50 95h

CuSO4 5,7 mg L-1 Cu

CuO 2500 mg L-1 Cu

Phosh 101 250 mg L-1 Cu

PVP-103 170 mg L-1 Cu

ASC-CuO ND

Acute toxicity ranking CuSO4> CuO(PVP)> CuO(prist)> CuO(powder)>CuO(ASC)

Cytotoxicity evaluation

CuO@ASC maintained the

antibacterial activity showing the

lowest toxicity with respect to

both reference samples and to

the modified ones

Inorganic NPs (CNR-ISTEC) Sol-gel technology

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Silica SiO2 core

Titania solutionTiO2 (anatase/rutile)

Silica core/Titania shell

Exposed Not exposed

Photocatalytic finish Without finish

SiO2/TiO2 NPs

Inorganic NPs (CeNTI)

Sol-gel technology

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

• Photocatalytic activity

• Antimicrobial activivty

• High washing fastness

•High whiteness level

•Maintenance of intrinsic textile properties

Samples Antimicrobial activity*

ASTM 2149-10 (% reduction)

Time of UV exposure 0h UV 1h UV

100% PES control 0% 7%

100% PES functionalised 62% 78%

67% CO/33% PES control 10% 13%

67%CO/33%PES functionalised 44% 65%

*Staphylococcus aureus ATCC 6538 strain

SiO2/TiO2 NPs

Inorganic NPs (CeNTI) Sol-gel technology

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

100 and 650 L reactors for NPs production

SiO2/TiO2 NPs

Inorganic NPs (CeNTI) Sol-gel technology

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Acyla

se+

Am

yla

se

Quorum quenching (acylase or lactonase)

70 %

inhibition

Matrix degradation (amylase)

Exopolysaccharides

In v

ivo

Enzymes for controlling bacterial biofilm

formation (UPC)

In v

itro

Silicone LbL Hybrid

QS signal

Acylase

30 %

inhibition

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Novel Antibacterial Nanospheres

•Quenching the quorum sensing

•Increased bacteria susceptibility to low concentration of antibiotic

Quorum quenching

acylase Gentamicin

US assisted generation of hybrid antibacterials

Antibacterial activity against

P. aeruginosa

Antibiofilm activity against

P. aeruginosa

100 % reduction

Hybrid acylase and gentamicin NPs were able to eradicate planktonic and biofilm growth of P. aeruginosa

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Function-Spacer-Lipids (SYN)

Function-Spacer-Lipid (FSL)

Architecture

Function

Spacer

Lipid

F groups with antibacterial potency: 1) spermine

2) selenium

3) aminoglycoside antibiotic

4)

-SeR

New, 2017

Se FSL-treated

S. aureus

Untreated

•FSLs with controlled structure and antimicrobial activity

•FSLs insert into bacterial membranes similar to natural glycolipids

•Coating of hydrophobic/hydrophilic surfaces without pre-treatment

•Coating by simple contact (10-60 s) with aqueous solution of FSL

•Coating with two of more anti-bacterial FSLs in a single-step process

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Polymer NPs (CNR-ISMAC)

Antimicrobial polypyrrol (PPy) with positive charges counter-balanced by counter-ions

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Simultaneous synthesis and deposition of PPy on fabrics by in situ oxidative polymerisation (4 h)

Polymer NPs

In Protect: separation of synthesis and deposition:

-High volume NPs production in batch mode

-Spontaneous NP formation during synthesis in water with anionic surfactants for NP

stabilisation

-Deposition of customised PPy NPs by the pilot machines

in situ

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Purpose From To What Date

Foreseen Interactions/internal deliverables

Brussels, Belgium Kick Off Meeting 23-24 January, 2017

Purpose Place Participants Date

Foreseen internal meetings