A Rigaku Miniflex 600 II (Rigaku, Tokyo, Japan) equipped with primary monochromated radiation (Cu K radiation source, λ = 1.54056 Å) available at UT Austin was adopted for XRPD study. Plasmid pCMV-β powder sample was loaded onto the sample holder and then analyzed in continuous mode. The operating conditions of accelerating voltage of 40 kV was at 15 mA, step size of 0.02◦ over a 2θ range of 5–40◦, scan speed of 1◦/min, and dwell time of 2 s as previously described [26 ].
Miniflex 600 2
Manufactured by Rigaku
Sourced in United States
The Miniflex 600 II is a compact X-ray diffractometer designed for phase identification and quantification of polycrystalline materials. It features a 600-watt X-ray source and a 1D semiconductor detector for fast data acquisition. The Miniflex 600 II is capable of recording X-ray diffraction patterns in the 2θ range of 5-60 degrees.
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5 protocols using miniflex 600 2
1
X-ray Powder Diffraction Analysis
2
Analyzing Crystallinity with X-ray Diffraction
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The crystallinity of the powders was evaluated using a benchtop X-ray diffraction instrument (Rigaku Miniflex 600 II, Woodlands, TX, USA) equipped with primary monochromated radiation (Cu K radiation source, λ = 1.54056 Å). The instrument was operated at an accelerating voltage of 40 kV at 15 mA. Samples were loaded in the sample holder and scanned in continuous mode with a step size of 0.02° over a 2θ range of 5–40° at a scan speed of 2°/min, and a dwell time of 2 s.
3
X-Ray Diffraction Characterization
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The XRD studies were conducted using a Rigaku MiniFlex 600 II (Rigaku Americas, The Woodlands, TX, USA) equipped with primary monochromated radiation (Cu K radiation source, λ = 1.54056 Å). The 2-theta angle was set at 5–40° (0.02° step, 1°/min, 40 kV, 15 mA).
4
X-Ray Powder Diffraction Analysis of API, PM, and KSD
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X-Ray powder diffraction (XRPD) analysis was conducted using a Rigaku MiniFlex600 II (Rigaku Americas Corporation, The Woodlands, TX, USA) instrument equipped with a Cu-Kα radiation source generated at 40 kV and 15 mA. The API, PM, and KSD samples were loaded into an aluminum pan, leveled with a glass slide, then analyzed in the 2-theta range between 2.5° and 35.0° while being spun. The step size was 0.02°, and the scanning rate was set to 5.0°/min. The following additional instrument settings were used: Slit condition: variable + fixed slit system; soller (incident): 5.0 degrees; IHS: 10.0 mm; DS: 0.625 degrees; SS: 8.0 mm; soller (receiving): 5.0 degrees; RS: 13.0 mm (open); and monochromatization: kb filter (×2). The data were collected using Miniflex Guidance software (Rigaku Corporation, Tokyo, Japan) and processed using PDXL2 software (Rigaku Corporation, Tokyo, Japan).
5
Preparation and Characterization of Niclosamide Amorphous Solid Dispersion
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The polymer Kollindon® VA64 (PVP–VA) and d -α-tocopheryl polyethylene glycol succinate (TPGS) were obtained from BASF, Germany. Niclosamide anhydrate was purchased from Shenzhen Nexconn Pharmatechs LTD (Shenzhen, China). In the preparation of niclosamide ASD, a PVP–VA–niclosamide–TPGS blend in a 60:35:5 ratio was ground using a mortar and pestle until the mixture was homogeneous. Then, the mixture was processed using a HAAKE MiniLab II Micro Compounder (Thermo Electron Corporation, Waltham, MA, USA) set at 150 rpm and 180 °C. Thereafter, the extrudate was milled using a Tube Mill Control (IKA, Staufen, Germany) and sieved to the range 45–125 µm. The solid-state characterization of the material was performed using powder X-ray diffraction (XRD) and differential scanning calorimetry (DSC). XRD studies were conducted using a Rigaku MiniFlex 600 II (Rigaku Americas, The Woodlands, TX, USA). The 2-theta angle was set at 5–40° (0.05° step, 2°/min, 40 kV, 15 mA). DSC was performed using a Model Q20 differential scanning calorimeter (TA Instruments, New Castle, DE, USA), increasing the temperature from 35 °C to 240 °C with a ramp temperature of 10 °C/min and a nitrogen purge of 50 mL/min.
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