DOI: 10.1039/C3CE42182A
Page 7 of 8
CrystEngComm
1. Detection wavelength in the UV–visible range was set at 339
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nm for FFA and 275 nm for TP. The samples were eluted with a
mobile phase containing a mixture of methanol and ultrapure
water in a ratio (v/v) of 60:40. Observed retention time for FFA is
3.896 min, for TP is 2.749, and for NA is 2.922 min. Prior to the
solubility and dissolution experiments, calibration plots for FFA,
TP, and cocrystals were constructed at a concentration range of
0.05 – 50 µg mL-1 and with R2 of 0.99 (n=3).
65
5
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Equilibrium solubility values were determined using the shake-
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10 flask method by stirring an excess amount of each sample in 5
mL of pH 7.5 buffer (with added 1 % tween 80) at 37 °C for 24
h. The solutions were filtered through 0.2 µm syringe filters, and
the concentration of the solutions was determined using HPLC.
IDR experiments were conducted using a Varian VK7010
15 dissolution apparatus equipped with a VK750D heater/circulator.
In each experiment, approximately 150 mg of sample was
compressed to a 0.5 cm2 disk in a rotating disk intrinsic
dissolution die using a hydraulic press at a pressure of 2 ton for 2
min. Only one side of the disk was exposed to the dissolution
20 medium and surface of the disk was constant throughout the
experiment. The intrinsic attachment was placed in a jar of 900
mL of phosphate buffer (pH 7.5) containing 1 % tween 80
preheated at 37 °C and stirring at 150 rpm. At regular time
intervals, 2 mL of the samples were withdrawn manually. The
25 collected samples were filtered through 0.2 µm nylon filters, and
assayed for FFA and TP concentrations using HPLC from the
respective calibration plots.
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a Crystallization and Particle Science, Institute of Chemical and
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40 † Electronic Supplementary Information (ESI) available: Melting point
data for the cocrystals and PXRD patterns of the powders obtained from
grinding experiments. See DOI: 10.1039/b000000x/
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