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See discussions, stats, and author profiles for this publication at: https://www.researchgate.net/publication/325066162 Thesis Presentation: Gold Nanoparticles for Enhanced Laser- Desorption Ionization of Biomolecules Presentation May 2018

SLIDE 1 See discussions, stats, and author profiles for this publication at: https://www.researchgate.net/publication/325066162

Thesis Presentation: Gold Nanoparticles for Enhanced Laser- Desorption Ionization of Biomolecules

Presentation · May 2018

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1 author: Some of the authors of this publication are also working on these related projects: AuNP for LDI-MS of Biomolecules View project Cody Sacks Penn State Hershey Medical Center and Penn State College of Medicine

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SLIDE 2

Gold Nanoparticles for Enhanced Laser-Desorption Ionization of Biomolecules

CODY SACKS, B.S. THE UNIVERSITY OF SCRANTON KATHERINE STUMPO, PH.D.

SLIDE 3

Presentation Overview

Background

Big Picture
MALDI-TOF MS
Matrices: DHB, AuNP

Data

Optimum M:A ratio
Peptides
Biomolecules
Steroids

Future Research Goals

SLIDE 4

MALDI-TOF Mass Spectrometry

ion source flight tube reflector sample plate reflector detector laser

KE = ½ mv2

SLIDE 5

SLIDE 6

Big Picture: AuNP vs. DHB as matrix

mass to charge ratio (m/z) relative abundance Ang I Ang III Sub P ACTH 1-17

SLIDE 7

Big Picture: AuNP vs. DHB as matrix

Bad DHB range Good DHB range Can AuNP improve spectra quality here? Ang I Ang III Sub P ACTH 1-17

SLIDE 8

2,5-Dihydroxybenzoic Acid (DHB)

Good matrix- transfers energy to analyte well

Conjugated system
Many protons

SLIDE 9

Gold Nanoparticles (AuNP)

Applications:

Targeted drug delivery
Tumor detection
Radiation sensitizer

Our research:

LDI-TOF matrix

https://news.brown.edu/articles/2013/10/nanogold http://file.scirp.org/Html/4-1190177_28878.htm

SLIDE 10

Mass Spectrometry Sample Preparation

DHB
3:1 acetonitrile:water (0.1% formic acid) @ 5.0 × 10-1 M
AuNP
2 nm and 5 nm AuNP obtained from Ted Pella, Inc.
concentrations of 1.5 × 1014 particles/mL, and 5 × 1013 particles/mL
Analytes
Dissolved into solvent @ 2.0 × 10-2 M
Final Solutions
Diluted to M:A of 104:1, 105:1, 106:1
Diluted to NP:A of 1:104, 1:105, 1:106

SLIDE 11

SLIDE 12

2 nm AuNP : cholesterol @ 1:105

AuNP = 20 Å Citrate layer = 3 Å Cholesterol layer = 71 Å

SLIDE 13

Optimum NP:A Ratio (vs. M/A Ratio)

10 20 30 40 50 60 70 80 90 100 %Int. 800 900 1000 1100 1200 1300 1400 1500 1600 1700 1800 1900 2000

m/z

280 mV 8.8 mV AngI5nm105_0001, AngI5nm1010_0001 Shimadzu Biotech Axima CFRplus 2.9.3.20110624 1318.86 1335.14 1204.61 1022.84 1159.66 1301.72 1004.54 1101.67 1258.55 875.65 904.54 1356.99 1946.63 1840.48 1703.82 1612.01 1494.40 1416.56 1660.33 1432.75 1683.71 1579.88

10 20 30 40 50 60 70 80 90 100 %Int. 800 900 1000 1100 1200 1300 1400 1500 1600 1700 1800 1900 2000

m/z

77 mV 11 mV AngI2nm105_0001, AngI2nm1010_0001 Shimadzu Biotech Axima CFRplus 2.9.3.20110624 1334.70 1318.64 1297.21 1341.02 985.09 1203.17 1301.61 1022.08 1118.44 800.14 943.56 1201.41 1384.68 1292.38 1545.73 1827.21 1733.83 1970.22 1636.62 1648.94

2nm AuNP 5nm AuNP

1:105 1:1010 NP:A

Ang I Ang I

SLIDE 14

Biomolecule Library

Compound Name Molecular Formula Molecular Weight (g/mol) Structure b-Lactose C12H22O11 340.3 Maltose C12H22O11 342.3 a-D Glucose pentacetate C16H22O11 390.34 Adenine HCl C5H5N5 · HCl · xH2O 135.13 Deoxycholic Adic C24H40O4 392.57 Cholesterol C27H46O 386.65 Cholic Acid C24H40O5 408.57 Taurocholic Acid C26H45NO7S 515.7058 Cholesteryl Acetate C29H48O2 428.69 Ouabain C29H44O12 584.652 Prednisone C21H26O5 358.428 Cortisone acetate C21H28O5 402.5 Proflavine C13H11N3 209.25 Diphenhydramine C17H21NO 255.355 D-glucogonic acid C6H12O7 196.16 Ibuprofen C13H18O2 206.29 Propyl Gallate C10H12O5 212.2 Triethanolamine C6H15NO3 149.19 Glycerophosphate (G3P) C3H9O6P 172.074 Berberine C20H18NO4+ 336.36122 Miconazole C18H14Cl4N2O 416.127 Gallic Acid C7H6O5 170.12

Analyte Formula 2 nm AuNP Observed Species 5 nm AuNP Observed Species -D-Glucose pentacetate C16H22O11 [M+Na]+, [M+K]+, [M+2K- H]+ [M+Na]+, [M+K]+ -D-Lactose C12H22O11 [M+H]+, [M+Na]+ [M+Na]+, F Cholic acid C24H40O5 [M+Na]+, [M+2Na-H]+ [M+Na]+, [M+2Na-H]+ Deoxycholic acid C24H40O4 [M+Na]+, [M+2Na-H]+, [M+K]+ [M+Na]+, [M+2Na-H]+ Diphenhydramine C17H21NO [M+H]+, [M+Na]+, [M+K]+, F+, [F+Au]+ [M+H]+, [M+Na]+, [M+K]+, [M+Au]+, F+, [F+Au]+ Maltose C12H22O11 [M+Na]+ [M+Na]+ Ouabain C29H44O12 [M+Na]+ [M+Na]+ Prednisone (cortisone) C21H26O5 [M+K]+, [M+Na]+ [M+Na]+ Taurocholic acid C26H45NO7S [M+2Na-H]+ [M+2Na-H]+ Cholesteryl acetate C29H48O2 [M+K]+, [M+Na]+ nd Cortisone acetate C21H28O5 [M+K]+ nd Ibuprofen C13H18O2 [M+Na]+ nd Propyl gallate C10H12O5 [M+H]+, [M+Na]+, [M+K]+ nd Cholesterol C27H46O nd [M+Na]+ Glycerol-3-phosphate C3H9O6P nd [M+H]+, [M+Na]+

22 compounds initially 15 compounds after initial analysis

7 molecules for no

difference in DHB vs. AuNP ionization or self-ionization

SLIDE 15

D-glucoronic acid: no significant difference

(A)DHB 106:1 (B)5 nm AuNP 1:105

SLIDE 16

Berberine: self-ionizing molecule

SLIDE 17

Cholesterol

(A) DHB 106:1 (B) 5 nm AuNP 1:106

SLIDE 18

Lactose

(A) DHB 106:1 (B) 5 nm AuNP 1:105

SLIDE 19

Diphenhydramine

(A) 2 nm AuNP 1:105 (B) 5 nm AuNP 1:105

SLIDE 20

Deoxycholic acid

(A) DHB 106:1 (B) 2 nm AuNP 1:104

[M-H+2Na]+

SLIDE 21

Cholic acid (ChA), Deoxycholic acid (dChA), and Taurocholic acid (TChA).

(A) DHB 105:1 (B) 5 nm AuNP 1:106

SLIDE 22

Cholic acid (ChA), Deoxycholic acid (DChA), and Taurocholic acid (TChA)

2 nm AuNP 1:105

DChA/ DChA/

SLIDE 23

Cholic acid, negative ion mode

(A) DHB 104:1 (B)2 nm AuNP 1:105

SLIDE 24

Future Goals

SHORT TERM Understand the fragmentation mechanism of steroids LONG-TERM Selective ionization Develop a library of molecule ionization patterns

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