2
0
2017
li
guo
1
journal
Original
Li, B.[Ben]
Guo, W.[Wei]
Ramsey, E. D.[Edward D.]
J. Chem. Eng. Data
2017
2020-09-29
Determining the Solubility of Nifedipine and Quinine in Supercritical Fluid Carbon Dioxide Using Continuously Stirred Static Solubility Apparatus Interfaced with Online Supercritical Fluid Chromatography
A high pressure vessel equipped with continuous magnetic stirring has been interfaced directly online with supercritical fluid chromatography (SFC). The interface consists of an oven housing a recirculation pump that maintains a constant flow of supercritical fluid solution from the vessel through a sample injection valve for online SFC analysis. The method involves increasing the vessel pressure in controlled steps to produce a series of progressively more saturated supercritical fluid carbon dioxide solutions for online SFC solubility measurements. The integrated static solubility system provides a convenient means to ensure equilibrium is established prior to performing online SFC solubility measurements and also facilitates a self-validation accuracy check procedure. For nifedipine, solubility data was obtained at 333.15 and 353.15 K through the pressure range from 12.5 to 27.5 MPa using 2.5 MPa steps. For quinine, solubility data was obtained at 323.15 and 343.15 K through the pressure range from 12.5 to 27.5 MPa using 3 MPa steps. All sets of experimental solubility data for each compound were correlated using the Mendez-Santiago and Teja model.
10.1021/acs.jced.7b00012
4
62
1530-1537
1
InChI=1S/C17H18N2O6/c1-9-13(16(20)24-3)15(14(10(2)18-9)17(21)25-4)11-7-5-6-8-12(11)19(22)23/h5-8,15,18H,1-4H3
HYIMSNHJOBLJNT-UHFFFAOYSA-N
dimethyl 4-(2-nitrophenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate
Nifedipine
C17H18N2O6
1
Commercial source
1
98
2
Stated by supplier
2
InChI=1S/C20H24N2O2/c1-3-13-12-22-9-7-14(13)10-19(22)20(23)16-6-8-21-18-5-4-15(24-2)11-17(16)18/h3-6,8,11,13-14,19-20,23H,1,7,9-10,12H2,2H3/t13-,14-,19-,20+/m0/s1
LOUPRKONTZGTKE-WZBLMQSHSA-N
quinine
(8.alpha.,9R)-6'-methoxycinchonan-9-ol
(8S,9R)-quinine
(R)-(6-methoxyquinolin-4-yl)((1S,2S,4S,5R)-5-vinylquinuclidin-2-yl)methanol
C20H24N2O2
1
Commercial source
1
99
2
Stated by supplier
3
InChI=1S/CO2/c2-1-3
CURLTUGMZLYLDI-UHFFFAOYSA-N
carbon dioxide
CO2
1
Commercial source
1
99.9
3
Stated by supplier
1
3
1
1
1
Principal objective of the work
EP
EP
3/8/2017
1
Mole fraction
Chromatography
1
Fluid (supercritical or subcritical phases)
Direct value, X
1
Data file compiler
Propagation of evaluated standard uncertainties
95
Fluid (supercritical or subcritical phases)
Crystal
1
1
Temperature, K
Fluid (supercritical or subcritical phases)
2
Pressure, kPa
Fluid (supercritical or subcritical phases)
1
333.15
5
2
12500
3
1
9.7e-06
2
1
1.2e-06
1
333.15
5
2
15000
2
1
1.31e-05
3
1
1.6e-06
1
333.15
5
2
17500
3
1
1.79e-05
3
1
2.2e-06
1
333.15
5
2
20000
1
1
2.32e-05
3
1
2.8e-06
1
333.15
5
2
22500
3
1
2.62e-05
3
1
3.2e-06
1
333.15
5
2
25000
2
1
3.1e-05
3
1
3.8e-06
1
333.15
5
2
27500
3
1
3.66e-05
3
1
4.4e-06
1
353.15
5
2
12500
3
1
7.9e-06
2
1
1e-06
1
353.15
5
2
15000
2
1
1.11e-05
3
1
1.4e-06
1
353.15
5
2
17500
3
1
1.99e-05
3
1
2.5e-06
1
353.15
5
2
20000
1
1
2.6e-05
3
1
3.2e-06
1
353.15
5
2
22500
3
1
3.52e-05
3
1
4.3e-06
1
353.15
5
2
25000
2
1
4.37e-05
3
1
5.3e-06
1
353.15
5
2
27500
3
1
5.36e-05
3
1
6.5e-06
2
3
1
2
1
Principal objective of the work
EP
EP
3/3/2017
1
Mole fraction
Chromatography
2
Fluid (supercritical or subcritical phases)
Direct value, X
1
Data file compiler
Propagation of evaluated standard uncertainties
95
Fluid (supercritical or subcritical phases)
Crystal
2
1
Temperature, K
Fluid (supercritical or subcritical phases)
2
Pressure, kPa
Fluid (supercritical or subcritical phases)
1
323.15
5
2
12500
3
1
1.53e-05
3
1
1.8e-06
1
323.15
5
2
15500
3
1
1.74e-05
3
1
2.1e-06
1
323.15
5
2
18500
3
1
2.27e-05
3
1
2.7e-06
1
323.15
5
2
21500
3
1
2.36e-05
3
1
2.8e-06
1
323.15
5
2
24500
3
1
2.86e-05
3
1
3.5e-06
1
323.15
5
2
27500
3
1
2.98e-05
3
1
3.6e-06
1
343.15
5
2
12500
3
1
1.2e-05
3
1
1.5e-06
1
343.15
5
2
15500
3
1
1.79e-05
3
1
2.2e-06
1
343.15
5
2
18500
3
1
2.35e-05
3
1
2.9e-06
1
343.15
5
2
21500
3
1
3.22e-05
3
1
3.9e-06
1
343.15
5
2
24500
3
1
3.98e-05
3
1
4.8e-06
1
343.15
5
2
27500
3
1
5.04e-05
3
1
6.1e-06