User:Roberta Diaz Jimenez/Notebook/CHEM 472/2016/02/10

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Objectives

  1. Setup AgNP and AuNP synthesis reactions for SPI, WPI, Casein, Pea Protein and Brown Rice Protein


Materials

  1. Used same nutritional proteins on 02/02/16
  2. Protein and gold stocks prepared fresh every day
  3. Ocean Optics UV Vis was used to record UVVIS Spectra of Casein AgNPs. The other machine broke and is unusable.
    1. Integration time= 10ms and Average =100.
    2. A water blank in the same quartz cuvette was subtracted from the spectra before running any samples.

Procedure

  1. Reducing stock protein concentrations (and thus concentrations in reaction mix) to increase metal/protein ratio to spur NP formation as we saw protein aggregate and nanofiber formation in previous reactions
  2. using citrate instead of fructose as reducing agent
  3. comparing citrate to no citrate samples, with citrate as only variable

Detailed Reaction Setup shown Below (4 hours 80˚C, 1ml rxns)

' Tube # 2.5mM HAuCl4 (µL) 4.375mMAgNO3 (µL) Protein (µL) 10 mM Citrate (µL) Water (µL) Au/Ag:Protein Notes
1 40 0 560 0 400 no change
.5mg/mL Casein 2 40 0 560 20 380
grams weighed: 5.06mg 3 40 0 200 0 760
Stock: 10mL 4 40 0 200 20 740
-reduce from 2mg/ml to .5mg/ml returning previous working concentration 5 0 40 560 0 400 all yellow soln, no particles
6 0 40 560 0 400 UV VIS
7 0 40 560 0 400
8 40 0 560 0 400 pink solutions w/ purple fibers on walls
9 40 0 560 20 380 pink soln with purple aggreagte on bottom
0.25mg/mL SPI 10 40 0 360 0 600 pink solution w/ purple fibers on walls
grams weighed: xmg 11 40 0 360 20 580 pink soln with purple aggreagte on bottom
Stock: xmL 12 40 0 200 0 760 pink soln with purple aggreagte on bottom
13 40 0 200 20 740 UV VIS pink soln with purple aggreagte on bottom
-change from 2/9/16, reduced concentration from .75mg/ml to .25mg/ml 14 0 40 560 0 400 No change 14-19
15 0 40 560 20 380
16 0 40 360 0 600
17 0 40 360 20 580
18 0 40 200 0 760
19 0 40 200 20 740
20 40 0 560 0 400 20-25 all pink solutions
21 40 0 560 20 380 some purple aggregate on walls
22 40 0 360 0 600
.25mg/mL Whey Protein 23 40 0 360 20 580
grams weighed: 10mg 24 40 0 200 0 760 purple aggregate at bottom of tube
Stock: 10mL 25 40 0 200 20 740 UV VIS
26 0 40 560 0 400 No change 26-31
-change from 2/9/16, reduced concentration from .75mg/ml to .25mg/ml 27 0 40 560 20 380
28 0 40 360 0 600
29 0 40 360 20 580
30 0 40 200 0 760
31 0 40 200 20 740
32 40 0 560 0 400 No change 32-37
33 40 0 560 20 380
0.25mg/mL Pea Protein 34 40 0 360 0 600
grams weighed: 10.38mg 35 40 0 360 20 580
Stock: 10.3mL 36 40 0 200 0 760
37 40 0 200 20 740
-dissolve in acid instead of base 38 0 40 560 0 400 38-43 all yellow soln, silver nanoparticles
39 0 40 560 20 380 UVVIS on All
40 0 40 360 0 600
41 0 40 360 20 580
42 0 40 200 0 760
43 0 40 200 20 740
44 40 0 560 0 400 no change
45 40 0 560 20 380 purple AUNPs
0.25mg/mL Rice Protein 46 40 0 360 0 600 no change
grams weighed: 10mg 47 40 0 360 20 580 purple AUNPs
Stock: 10mL 48 40 0 200 0 760 no change
49 40 0 200 20 740 UVVIS Purple AUNPs
-this needs to be dissolved by base, particles float to the bottom 50 0 40 560 0 400 no change
-Did not dissolve. We didn't add* try next week 51 0 40 560 20 380 slightly yellow
52 0 40 360 0 600 no change
53 0 40 360 20 580 slightly yellow
54 0 40 200 0 760 no change
55 0 40 200 20 740 slightly yellow


Results

Figure 1: UVVis Spectra for Pea Protein AgNP Samples With and Without Citrate (synthesized on 02/10/2016)
800px


Figure 2: UVVis Spectra for Casein AgNP Samples in Triplicate (synthesized on 02/10/2016)
2.10.16caseinAgNP.png


Figure 3: UVVis Spectra for WPI AuNP Samples by Protein Concentration (synthesized on 02/010/2016)
2.10.16 WPI AuNP.png

-Only 2 of the WPI-Au samples with citrate formed nanoparticles, the WPI-Au samples without citrate formed nanofibers which clung to walls.

Figure 4: AuNP UV-Vis Spectra for our Red AuNPs (synthesized on 02/10/2016)
2.10.16SPIAuNP.png

-This shows UVVIS Spectra for SPI-Au sample with lowest protein concentration tested and highest concentration of citrate. All other SPI-Au samples formed protein aggregate, fibers or both.