Data of preparation and evaluation of supramolecular hydrogel based on cellulose for sustained release of therapeutic substances with antimicrobial and wound healing properties

The data article refers to the paper “supramolecular hydrogel based on cellulose for sustained release of therapeutic substances with antimicrobial and wound healing properties”[1]. The dataset includes the synthesis and characterization of (E)-1,3-bis(4-(allyloxy)phenyl)prop‑2-en-1-one (3) (crosslinking agent). Moreover, the multiwall carbon nanotubes (MWCNTs) synthesis and functionalization (MWCNTs-COOH) are described. The formulation obtained by adding multiwalled carbon nanotubes-COOH with the crosslinked cellulose-chalcone hydrogel is abbreviated as MWCNTsCCH, and the same formulation loaded with therapeutic substances (TS) is named MWCNTsCCH-TS. The MWCNTsCCH database such as components and their amounts, swelling degree, thermogravimetric analysis, and cytotoxicity evaluation are depicted. Finally, to elucidate the mechanism of therapeutic substances release, the obtained averages of the release profiles were fitted through mathematical models.

apeutic substances release, the obtained averages of the release profiles were fitted through mathematical models.
© 2020 The Author(s). Published by Elsevier Inc. This is an open access article under the CC BY license.

Organic Chemistry Specific subject area
Preparation, characterization and evaluation of supramolecular hydrogel based on cellulose Type of data Table  Image Graph Figure  Filtered data Raw data How data were acquired Mass spectrometry experiments . These analyses were carried out on a high-resolution high accuracy hybrid double quadrupole (Qq) and orthogonal time-of-flight (Tof) mass spectrometer (QTof, Micromass UK). The temperature of the nebulizer was 50 °C. The ESI source and the mass spectrometer were operated in the positive-ion mode. FT-IR: Fourier transform infrared spectroscopy (NEXUS 670 FT-IR, Thermo Nicolet, Madison, WI, USA). Samples for FT-IR measurements were prepared by grinding dry material into KBr in an agate mortar at a very low concentration of compound 3 (0.03 wt%). The wavenumber range scanned was 40 0 0-40 0 cm −1 ; 32 scans of 2 cm −1 resolution were signal-averaged and stored. NMR . The 1 H NMR and 13 C NMR spectra were recorded on a Bruker (400 MHz) spectrometer. Chemical shifts ( δ) are recorded in ppm with the solvent resonance as the internal standard and coupling constants (J) recorded in Hz. Equilibrium swelling ratio of MWCNTsCCH: The water uptake activity was calculated by the equilibrium swelling ratio (% ESR). The ESR of the hydrogel samples was estimated according to the following equation: x 100% TGA : thermogravimetric analyzer STD 650 TA-235 instruments by TA-instruments. ≈ 3 mg of freeze-dried sample was placed into the balance and were heated to a constant heating rate of 10 °C min −1 . The heating was realized from room temperature to 800 °C in N 2 or air as a reactive gas (with a mass flow of 50 mL min −1 .), which was switched when the temperature reached 800 °C, and hold at this temperature during 30 min, for allowing the oxidation process. Also, 50 mL min −1 of N 2 was used as protection gas into the electronic balance; around 3 mg of the composite was placed into a Pt crucible for each analysis. HPLC: Perkin Elmer series 200 HPLC system (Norwalk, CT, USA) with a UV-vis detector. A YWG C-8 (250 mm x 4.6 mm i.d. x 10 μm) column was utilized for the sample analysis. Cytotoxicity and cell viability . The data were acquired from fibroblast MTT assay.

Data format
Raw data of models: Microsoft Excel; GraphPad Prism 8

Parameters for data collection
According to the respective experimental measurements, some data were acquired at specific intervals during a period of time and other data were collected at a specific pH and temperature.
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Description of data collection
The data for structural characterization of compound 3 was obtained by 1 H-13 C NMR, FT-IR and time-of-flight mass spectrometry analysis.

Value of the Data
The data presented is useful to know the behavior release if therapeutic substances from carbon nanotube-containing cellulose-chalcone hydrogels, with the goal of achieving multiple therapeutic effects.
The beneficiaries of these data are researchers who investigate the release of multiple drugs from polymeric matrices of cellulose-based hydrogels.
The data presented will allow the development of new polymeric platforms of cellulosebased hydrogels, being a guide for the determination of the behavior of these compounds for the release of multiple drugs.

Data description
The synthesis of crosslinker (E) −1,3-bis(4-(allyloxy)phenyl)prop-2-en-1-one ( 3 ) is represented in Fig. 1 and detailed description of the reaction procedure is stated in the experimental design, materials, and methods section. The compound 3 was characterized by TOF mass and FTIR spectroscopy analysis (see Figs. 2 and 3 ). The preparation of MWCNTsCCH and loading of therapeutic substances (MWCNTsCCH-TS) are depicted in Table 1 and detailed synthesis is ex-  The weight percentage of Chalcone, MWCNTs, and TSs is in relation to the cellulose mass.  Table 2 ). Graphs of the study results were designed by utilizing GraphPad Prism 6. Statistical significance was set at p < 0.05. The mass loss (TG) and derivative (DTG) curves were obtained in the interval of room temperature to 800 °C, this data are showed in Table 3 . The release percentage of linezolid, allantoin, dexpanthenol, and resveratrol from MWCNTsCCH are shown in Table 4 . These data allow obtain the release profile and to calculate release kinetic of TS. To elucidate the mechanism of TS release, the data of Table 5 were obtained by applying different mathematical modeling drug-release equations, namely, zero-order ( Eq. (3) ), first-order ( Eq. (4) ), Hixson-Crowell ( Eq. (5) ), Higuchi ( Eq. (6) ), Korsmeyer-Peppas ( Eq. (7) ), and Peppas-Sahlin ( Eq. (8) ) equations [2][3] . Fig. 5 and Table 6 demonstrates the CNTs-CCH cytotoxicity. This experiment was carried out to measure fibroblast cell viability after exposure to MWCNTsCCH. The biocompatibility of sterilized MWCNTsCCH after 24 h was evaluated by a cell viability assay using L929 fibroblast    Percentage of cell viability obtained from the MTT assay of the L929 fibroblast cells with respect to negative control (without MWCNTsCCH). Each bar indicates mean ± relative standard deviations (RSD) of three replications. Bars not labeled by the same letter represent statistical significance at P ≤ 0.05 using ANOVA followed by Tukey's HSD test. cells. Fig. 5 shows the fibroblast cell viability in the presence of three different concentrations of MWCNTsCCH (500, 1500, and 2500 μg mL −1 ) .
During the isothermal oxidation at 800 °C under air atmosphere, the consumption of the high graphitized carbon takes place. These results show how the functionalization of the MWCNTs-COOH surface affects this graphitization process and therefore its oxidation resistance.

Multiwall carbon nanotubes (MWCNTs) synthesis and functionalization (MWCNTs-COOH)
MWCNT were obtained through an ethanol decomposition reaction process at 900 °C in presence of perovskite-like oxide (LaFeO 3 ) as a catalyst precursor by following the previously reported study [5] . The catalyst was placed into a horizontal reactor after which temperature was raised at 10 °C • min −1 under N 2 atmosphere until the desired reaction temperature. Then ethanol at a 50% of volumetric fraction was injected over 4 h. Obtained MWCNTs were treated with 65% HNO 3 and 96% H 2 SO 4 (3:1), for 15 min at 130 °C, by applying a power of 500 W in a Milestone MicroSYNTH microwave reactor. The product was then filtered using a 0.45 μm pore size mixed cellulose-ester filter (advantec MFS, Inc.) and washed with deionized water until neutral pH. Filtered MWCNTs-COOH were dried at 100 °C for 24 h. This MWCNTs-COOH was characterized through different analytical techniques such as exhibited below [6] . The MWCNTs-COOH was termed as MWCNTs.

Equilibrium swelling ratio of MWCNTsCCH
The water uptake activity was calculated by the equilibrium swelling ratio (% ESR) at specific time intervals, according to the protocol of Marican, et al. 2018 [7] . The MWCNTsCCH film was placed in phosphate-buffered saline (PBS) (pH 7.4) and acetate buffer (pH 4.0) at ∼25 °C for 48 h until swelling equilibrium was reached. The weight of the wet sample [W w (g)] was measured after cautiously removing surface moisture with absorbent paper. The weight of the dried sample [W d (g)] was obtained after freeze-drying the prepared hydrogel. The ESR of the hydrogel samples was estimated according to the following equation ( Eq. (1) ): (1)

Thermogravimetric analysis
The sample analyses of MWCNTs and MWCNTsCCH were performed in a thermogravimetric analyzer (STD 650 TA-235, TA Instruments). Approximately 3 mg of freeze-dried sample was placed into the instrument balance and heated at a constant heating rate of 10 °C min −1 . The heating was conducted from room temperature to 800 °C in N 2 or air as a reactive gas (with a mass flow of 50 mL min −1 ). The temperature was held at 800 °C for 30 min to allow the oxidation process to complete. Additionally, 50 mL min −1 N 2 was used as the protection gas in the electronic balance. Approximately 3 mg of the composite was placed into a platinum crucible for each analysis. The first region of the thermal analysis, from room temperature to 800 °C under an N 2 atmosphere, examines the thermolabile molecules or fragments that can be decomposed by simple heating of the samples, such as the functional groups over the carbon nanotubes. The second region, the oxidative process (under O 2 ), aims to observe the sample's oxidative resistance under extreme conditions, reactive gas (dynamic air atmosphere) and high temperature (800 °C). For the second region, once the temperature reaches 800 °C, the gas through the sample was switched to air (50 mL min −1 ), maintaining during all time the protective atmosphere across the electronic balance (50 mL min −1 of N 2 ) and keeping the temperature isothermally at 800 °C.

Preparation of MWCNTsCCH and loading of therapeutic substances
First, 1 g of the cellulose solution was mixed with chalcone (CH) ( 3 ) at 20 w/w%. The synthesis and characterization of CH are shown in this data article, Section 2.1 and Figs. 1 , 2 and 3 . The reaction mixture was continuously sonicated for 2 h (the temperature of the sonication bath ranged from 25 to 60 °C) according to the modified method from Cass, et al. 2010 [8] . Then, a yellow viscous liquid corresponding to the crosslinked cellulose-chalcone prehydrogel was obtained. Second, MWCNTs (15 w/w%, MWCNTs-COOH, average size (diameter × length): 20-80 nm × 10-15 μm) were mixed with the prehydrogel and sonicated for 2 h at 50 °C. Next, the homogenized black mixture (prehydrogel-MWCNTs) was dialyzed for 2 days. Then, the therapeutic substances (TSs) allantoin, dexpanthenol, resveratrol, and linezolid were added to the solution [9] . The resulting mixture was sonicated for 2 h at 50 °C until a homogenized solution was obtained. Finally, the mixture solution was placed in an oven at 45 °C overnight until the crosslinking was complete and the hydrogel film was formed. The final composition of the loaded hydrogel is depicted in Table 1 .

Drug release kinetics from MWCNTsCCH-TS
The protocol was performed according to Forero-Doria, et al., 2020 [1] . A known mass of MWCNTsCCH-TS (400 mg of dry sample) was placed in a flask, and 5 mL of PBS (pH 7.4) was poured over the formulation as a release medium. The flask was moved to an orbital shaker incubator water bath (Farazteb, Iran) at 33.5 ± 0.1 °C (skin temperature) and shaken at 35 ± 2 rpm. After every time interval, the PBS was recovered and replaced with an equal volume to maintain sink conditions during all studies. The samples and controls were analyzed by a Perkin Elmer series 200 HPLC system (Norwalk, CT, USA) with a UV-Vis detector. A YWG C-8 (250 mm into the HPLC apparatus. Isocratic elution with methanol/water (50:50, v/v) at a constant flow rate of 1.0 mL min −1 was used as the mobile phase. The analytical wavelength was 254 nm at room temperature. The release rate of MWCNTsCCH-TS was obtained by applying the concentration of released and loaded TSs to the following correlation ( Eq. (2) ): Cumulative TS release ( % ) = Cumulative amount of TS released × 100 Initial amount of TS (2) Drug release kinetics were carried out by applying different mathematical modeling drugrelease equations, namely, zero-order ( Eq. (3) ), first-order ( Eq. (4) ), Hixson-Crowell ( Eq. (5) ), Higuchi ( Eq. (6) ), Korsmeyer-Peppas ( Eq. (7) ), and Peppas-Sahlin ( Eq. (8) ) equations: where Q t is the amount of drug released at time t, and Q 0 is the original drug concentration in the hydrogel.
where C t is the amount of drug released in time t , C 0 is the initial amount of drug in the tablet, and K is the rate constant.
where Q is the cumulative drug release, K is the Higuchi release constant, and t is the time where M t /M is the cumulative drug release, K is the release constant, t is the time, and n is the release exponent.
where M t and M ∞ are the absolute cumulative amounts of drug release at time t and at infinite time, respectively.