The samples were subjected to differential scanning calorimetry (DSC) and thermogravimetry (TG) analyses, both carried out in triplicate. Approximately 10 mg of sample were placed in an aluminum straw for DSC analysis (Mettler DSC 823e System, Mettler Toledo, Spain), at a heating rate of 15 °C/min in N2 atmosphere, from 25 to 350 ± 1 °C temperature. For TG analysis (TA-50WSI, SHIMATZU, 50WSI, Tokyo, Japan), approximately 10 mg of sample were placed in an aluminum straw and analyzed at 10 °C/min heating rate in N2 atmosphere with a temperature range of 25 to 500 ± 1 °C [18 (link)].
Dsc 823e system
Manufactured by Mettler Toledo
Sourced in Spain
The DSC 823e System is a thermal analysis instrument used for differential scanning calorimetry (DSC) measurements. It is designed to analyze phase transitions, thermodynamic properties, and thermal stability of a wide range of materials.
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5 protocols using dsc 823e system
1
Thermal Properties of Materials
2
Physicochemical Characterization of PGZ-NPs
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To determine the physical state of the PGZ-NPs and their interactions with any compound of the formulation, studies by Differential Scanning Calorimetry (DSC), X-ray spectroscopy, and Fourier Transform Infrared (FTIR) were performed before and after the spray drying process.
DSC analysis was performed using a DSC 823e System (Mettler Toledo, Barcelona, Spain). The temperature was calibrated by the melting transition point of indium (purity ≥ 99.95%; Fluka, Switzerland) prior to sample analysis. The DSC measurements used a heating ramp from 30 to 240 °C at 10 °C/min in a nitrogen atmosphere. Data were evaluated using the Mettler STARe V 9.01 dB software (Mettler Toledo, Barcelona, Spain).
To determine the state—crystalline or amorphous—of the samples, X-ray spectral measurements were performed using Siemens D500 system (Karlsruher, Germany). X-ray powder diffractograms were recorded using a Cu Kα2 radiation (45 kV, 40 mA, λ = 1.544 Å) in the range (2θ) from 2° to 60° with a step size of 0.026° and the measuring time was 200 s per step.
FTIR spectra were achieved using a Thermo Scientific Nicolet iZ10 with an ATR diamond and DTGS detector (Thermo Fischer Scientific, Waltham, MA, USA). The scanning range used was 500–4000 cm−1.
DSC analysis was performed using a DSC 823e System (Mettler Toledo, Barcelona, Spain). The temperature was calibrated by the melting transition point of indium (purity ≥ 99.95%; Fluka, Switzerland) prior to sample analysis. The DSC measurements used a heating ramp from 30 to 240 °C at 10 °C/min in a nitrogen atmosphere. Data were evaluated using the Mettler STARe V 9.01 dB software (Mettler Toledo, Barcelona, Spain).
To determine the state—crystalline or amorphous—of the samples, X-ray spectral measurements were performed using Siemens D500 system (Karlsruher, Germany). X-ray powder diffractograms were recorded using a Cu Kα2 radiation (45 kV, 40 mA, λ = 1.544 Å) in the range (2θ) from 2° to 60° with a step size of 0.026° and the measuring time was 200 s per step.
FTIR spectra were achieved using a Thermo Scientific Nicolet iZ10 with an ATR diamond and DTGS detector (Thermo Fischer Scientific, Waltham, MA, USA). The scanning range used was 500–4000 cm−1.
3
Physicochemical Characterization of DXI Nanoparticles
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Differential scanning calorimetry (DSC) analysis was performed using a DSC 823e System Mettler-Toledo, Barcelona, Spain. A pan with indium (purity ≥99.95%; Fluka, Switzerland) was used to check the calibration of the calorimetric system. An empty pan served as a reference. The DSC measurements were carried out in all DXI NPs formulations using a heating ramp from 25 to 105 °C at 10 °C/min in a nitrogen atmosphere. Data was evaluated using the Mettler STARe V 9.01 dB software (Mettler-Toledo, Barcelona, Spain) [5 (link)].
X-ray spectroscopy (XRD) was used to analyze the amorphous or crystalline state of the samples (centrifuged DXI NPs). Samples were sandwiched between 3.6 μm polyester films and exposed to CuKα radiation (45 kV, 40 mA, λ = 1.5418 Å) in the range (2θ) of 2–60° with a step size of 0.026° and a measuring time of 200 s per step [13 (link)].
Fourier transform infrared (FTIR) spectra of DXI NPs were obtained using a Thermo Scientific Nicolet iZ10 with an ATR diamond and DTGS detector (Barcelona, Spain) [12 (link)].
X-ray spectroscopy (XRD) was used to analyze the amorphous or crystalline state of the samples (centrifuged DXI NPs). Samples were sandwiched between 3.6 μm polyester films and exposed to CuKα radiation (45 kV, 40 mA, λ = 1.5418 Å) in the range (2θ) of 2–60° with a step size of 0.026° and a measuring time of 200 s per step [13 (link)].
Fourier transform infrared (FTIR) spectra of DXI NPs were obtained using a Thermo Scientific Nicolet iZ10 with an ATR diamond and DTGS detector (Barcelona, Spain) [12 (link)].
4
Characterization of Thermosensitive Nanoparticles
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Interaction studied were carried out by previous ultracentrifugation of the samples at 15,000 rpm during 30 min of TH-NPs (Beckmann-Coulter ultracentrifuge). The possible interactions between TH and PLGA were assessed by differential scanning calorimetry (DSC). Thermograms were obtained on a DSC823e System (Mettler-Toledo, Barcelona, Spain). A pan with indium (purity ≥ 99.95%; Fluka, Switzerland) was used to check the calibration of the calorimetric system and an empty pan was used as a reference [25 (link)]. Samples were heated from 10 °C to 100 °C at 5 °C/min under a nitrogen atmosphere. Data were evaluated from the peak areas with Mettler STARe V 9.01 DB software (Mettler-Toledo). The physical state (amorphous or crystalline) of TH and TH-NP was analyzed by X-ray diffraction (XRD). Samples were sandwiched between 3.6 µm films of polyester and exposed to Cu K α radiation (λ = 1.5418 Å) with work power (45 kV, 40 mA). Diffractograms were recorded on a PANalytical X’Pert PRO MPD θ/θ, powder diffractometer of 240 mm of radius, using PIXcel detector (active length = 3.347°). The measure time was defined 200 s per step, 2θ/θ scans from 2 to 60°2θ with a step size of 0.026°2θ [49 (link)].
5
Physicochemical Characterization of PGZ-Loaded Nanoparticles
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To assess the physical state of the PGZ and the possible interactions between the drug and the polymer, X-ray spectroscopy came into play, backed by FTIR spectral measurements and differential scanning calorimetry (DSC) analysis.
X-ray spectroscopy was used to analyse the state (amorphous or crystalline) of the PGZ-NSs. Powder of PGZ, PLGA-PEG, and NSs was sandwiched between films of polyester and exposed to CuK" radiation (45 kV, 40 mA, λ = 1.5418 Å) in the range 2ϴ/ϴ scands from 2º to 60º 2ϴ with a step size of 0.026º 2ϴ. The measuring time was 200 seconds per step.
To obtain FTIR spectra of PGZ, PLGA-PEG, and NSs a Thermo Scientific Nicolet iZ10
with an ATR diamond and DTGS detector were used. The scanning range was 525-4000 cm -1 .
DSC analysis was performed using a DSC 823e System (Mettler-Toledo, Barcelona, Spain). A pan with indium (purity ≥ 99.95 %; Fluka, Switzerland) proved ideal to check the calibration of the calorimetric system. An empty pan served as a reference. The DSC measurements were carried out on the PGZ, PLGA-PEG and NSs. On heating the samples (2.32-2.95 mg) from 25 ºC to 235 ºC at 10 ºC/min in a nitrogen atmosphere it was possible to evaluate the data from the peak areas using the Mettler STARe V 9.01 DB software (Mettler-Toledo).
X-ray spectroscopy was used to analyse the state (amorphous or crystalline) of the PGZ-NSs. Powder of PGZ, PLGA-PEG, and NSs was sandwiched between films of polyester and exposed to CuK" radiation (45 kV, 40 mA, λ = 1.5418 Å) in the range 2ϴ/ϴ scands from 2º to 60º 2ϴ with a step size of 0.026º 2ϴ. The measuring time was 200 seconds per step.
To obtain FTIR spectra of PGZ, PLGA-PEG, and NSs a Thermo Scientific Nicolet iZ10
with an ATR diamond and DTGS detector were used. The scanning range was 525-4000 cm -1 .
DSC analysis was performed using a DSC 823e System (Mettler-Toledo, Barcelona, Spain). A pan with indium (purity ≥ 99.95 %; Fluka, Switzerland) proved ideal to check the calibration of the calorimetric system. An empty pan served as a reference. The DSC measurements were carried out on the PGZ, PLGA-PEG and NSs. On heating the samples (2.32-2.95 mg) from 25 ºC to 235 ºC at 10 ºC/min in a nitrogen atmosphere it was possible to evaluate the data from the peak areas using the Mettler STARe V 9.01 DB software (Mettler-Toledo).
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