Supporting Information for. Effect of complementary small molecules in the properties of bicomponent. hydrogel of riboflavin
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1 Supporting Information for Effect of complementary small molecules in the properties of bicomponent hydrogel of riboflavin Abhijit Saha, Bappaditya Roy, Aluri Esterrani and Arun K. Nandi * Polymer Science Unit, Indian Association for the Cultivation of Science, Jadavpur, Kolkata , India for correspondence, psuakn@iacs.res.in 1
2 Supporting Scheme SS1: Chemical structures of riboflavin, acetoguanamine, salicylic acid and 3,5- dihydroxy benzoic acid. OH OH OH OH OH N N O HO N O NH O OH Riboflavin (R) 3,5-dihydroxy benzoic acid (B) HO N HO H 2 N N N O Salicylic acid (S) NH 2 Acetoguanamine [2,4- diamino-6-methyl-striazine (D)] 2
3 Supporting Table ST1: Life time and relative amplitude values of pure R solution and RS11, RD11 gels at same concentration of R at 30 0 C. Av. Systems Life (ns) (ns) (ns) time (a 1 ) (a 2 ) (a 3 ) (ns) Pure R RS RD
4 Supporting Figure S1: Polarised optical micrograph of hydrogel of (a) RS11 (1 % w/v) & (b) RB11 (1% w/v); FESEM micrographs of xerogels of above (c) RS11 and (d) RB11 hydrogels. a c 0.5 mm 10 M d b 0.5mm 10 M 4
5 Supporting Figure S2: DSC thermograms of (a) RB11 (b) RD11 and (c) RS % hydrogels (10 0 C/min heating and 5 0 C/min cooling rates). (a) 1st Heating 66 0 C Heat flow (Endo Up) Cooling 2nd Heating C C Temperature( 0 C) (b) 1st Heating C (c) C 1st Heating Heat flow (endo up) Cooling C 2nd Heating C Heat flow (endo-up) Cooling 2nd Heating C C Temperature( 0 C ) Temperature( 0 C) 5
6 Supporting Figure S3: DSC thermograms of gels at indicated compositions (% W/V) prepared after homogenization at 90 0 C and then keeping at 30 0 C for 1day (heating rate of 10 0 / min): (a) RS11 gels, (b) RD11 gels and (c) RB11 gels. (a) RS11 5 % 70 0 C C Heat flow ( Endo up ) 3.5 % 2.5 % 1 % C C Temperature 0 C (b) RD11 5 % C C Heat Flow ( Endo - Up ) 3.5 % 2.5 % 1 % C C Temperature ( 0 C ) 6
7 (c) RB C Heat Flow ( Endo up ) 5 % 3.5 % 2.5 % 1 % 63 0 C C 66 0 C Temperature ( 0 C ) 7
8 Supporting Figure S4. (a) Storage (G ) and loss (G ) modulus vs. frequency plot and (b) Storage modulus (G ) vs % strain plot of RD G'(1) Storage modulus (G') - Pa G'(2) G'(3) G''(1) G''(2) Loss modulus (G'') - Pa G''(3) Angular Frequency (ω) - rad/sec 8
9 Supporting Figure S5: FTIR spectra of xerogels of (a) RS11 (b) RB11 and (c) RD11along with the pure components R, B, D and S. (a) R 1734 % Transsmission RS11 S Wave number (cm -1 ) (b) R 1734 % Transmssion RB B Wave number (cm -1 )
10 (c) R 1734 % Transmission RD D Wave number(cm -1 ) 10
11 Supporting Figure S6: 1H NMR spectrum of R in D2O. R 11
12 Supporting Figure S7: 1H NMR spectrum of B, RB11 gel and RB11 sol in D2O. B RB11 1% Gel RB11 sol 12
13 Supporting Figure S8: 1 H NMR spectrum of S, RS11 gel and RS11 sol in D 2 O. S RS11 1% Gel RS11 Sol 13
14 Supporting Figure S9: 1 H NMR spectrum of D, RD11 gel and RD11 sol in D 2 O. D RD % Gel RD11 sol 14
15 Supporting Figure S10. WAXS patterns of xerogels of RB11, RS11 and RD11 with pure R, B, S and D. R RB11 B RS11 RD θ D S 15
16 Supporting Figure S11: Comparison XRD spectra of xerogels and hydrogels of RB11, RS11 and RD11 systems at 30 0 C. RB11 system Intensity (cps) H ydrogel Xerogel W avelength (nm ) RS11 System Intensity (cps) H ydrogel Xerogel W avelength (nm ) RD11 System Intensity (cps) H ydrogrel Xerogrel W avelength (nm ) 16
17 Supporting Figure S12: (a) UV-vis spectra of RS complex sols, pure R and pure S in solution (at 0.01 % w/v concentration) and (b) plot of absorbance at 445 nm vs. mol fraction of R in different RS complexes. (a) Absorbance R RS11 RS12 RS13 RS14 RS21 RS312 RS31 RS41 RS412 S Wavelength (nm) (b) RS Absorbance (a. u.) Mol fraction R in complex 17
18 Supporting Figure S13: (a) UV-vis spectra of RB complex sols, pure R and pure B in solution (at 0.01 % w/v concentration) and (b) plot of absorbance at 445 nm vs. mol fraction of R in different RB complexes. (a) Absorbance (a. u.) Wavelength (nm) (b) RB Absorbance (a. u.) B RB11 RB12 RB13 RB14 RB21 RB31 RB41 R Mol fraction R in complex 18
19 Supporting Figure S14: Time-resolved fluorescence decay of (a) R (b) RD11 gel and (c) RS11 hydrogel at 25 0 C (λ ex =375 nm). The sharp profile on the left is the lamp profile. (a) Count (log) Pure R in Solution Probe Decay Fit Time (nanosecond) (b) Counts (log) RD11 1% Gel Probe Decay Fit Time (nanosecond) 19
20 (c) RS11 Probe Decay Fit Counts (log) Time (nanosecond) 20
21 Supporting Figure S15: Fluorescence spectra of RS11 1% (a and b) and RB11 1% (c and d) gel at different ph (4, 5, 6.7, 8 and 9.2) and Temperature ( C). (a) 5x10 6 ph 6.7 4x10 6 ph 5 Intensity (cps) 3x10 6 2x10 6 1x10 6 ph 8 ph 9.2 ph Wavelength (nm) (b) 6x10 6 5x C 35 0 C 25 0 C RS11 Intensity (cps) 4x10 6 3x10 6 2x C 65 0 C 75 0 C 1x Wavelength (nm) Figure 11 21
22 (c) 2.0x10 6 ph x10 6 ph 5 Intensity (cps) 1.0x x10 5 ph 8 ph ph Wavelength (nm) (d) 4x10 6 3x C 45 0 C 35 0 C Intensity (cps) 2x10 6 1x C 65 0 C 75 0 C Wavelength (nm) 22
23 Supporting Figure S16: Comparison of PL- spectra of dried gels of RD11, RB11 and RS11 systems (Inset PL spectra of pure R) at 30 0 C. 5x x Intensity ( cps ) 4x10 5 3x10 5 2x10 5 Intensity (cps) 5.0x Wavelength (nm) 583 RD11 RB11 RS x Wavelength (nm) 23
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