jssc3671-sup-0001-SuppMat

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Simultaneous
determination
of
aliskiren
hemifumarate,
amlodipine
besylate
and
hydrochlorothiazide in their triple mixture dosage form by capillary zone electrophoresis
Mohamed Salim a,b*, Walid M. Ebeid
Gabor Patonay a
a,c
, Nahed El-Enany b, Fathalla Belal
a
b
, Mohamed Walash
b ,
Department of Chemistry, Georgia State University, P.O. Box 4098, Atlanta, Georgia 30302-4098,
USA.
b
Department of Analytical Chemistry, Faculty of Pharmacy, University of Mansoura, P.O. Box 35516,
Mansoura, Egypt
c
Pharmaceutical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr El-Aini St.,
Cairo 11562, Egypt.
Page S-1
Table OF Contents.
Title
Page
Figure S-1.
Effect of buffer pH on separation of the studied drugs.
S-3
Figure S-2.
Effect of buffer conc. on separation of the studied drugs.
S-3
Figure S-3.
Effect of organic modifiers on separation of the studied drugs.
(A) methanol (B) ethanol
(C) acetonitrile.
S-4
Figure S-4.
Effect of applied voltage (kV) on separation of the studied drugs.
S-5
Figure S-5.
Effect of injection time (sec) on separation of the studied drugs.
S-5
Figure S-6.
Effect of capillary cartridge temperature (◦C) on separation of the
studied drugs.
S-6
Figure S-7.
Selection of the detection wavelength.
S-6
Figure S-8.
Application of the proposed method for the simultaneous
determination of the studied drugs in Amturnide® tablets (7.5 g/ml of
AML, 179.25 g/mL ALS, 13.5 g/mL HCZ and 25 g/mL MXP)
under the optimized conditions.
S-7
Figure S-9.
Application of the proposed method for the simultaneous
determination of synthetic mixture of 8 g/ml of AML, 240 g/mL
ALS, 20 g/mL HCZ and 25 g/mL MXP under the optimized
conditions.
S-7
Tables S-1.
Performance data for the determination of the studied drugs by the
proposed CZE method.
S-8
Tables S-2.
Robustness data for the determination the studied drugs by the
proposed CZE method.
S-9
Tables S-3.
Assay results for the determination of the studied drugs in their
synthetic mixture and comparison methods.
S-10
Page S-2
160000
140000
Absorbance (mAU)
120000
100000
pH 7.0
80000
pH 6.5
60000
pH 6.0
40000
pH 5.5
20000
pH 5.0
0
-20000 0
2
4
6
8
10
Time (min)
12
14
16
18
20
Figure S1.
160000
140000
Absorbance (mAU)
120000
100000
50 mM, 53 µA
80000
40 mM, 41 µA
60000
30 mM, 31 µA
40000
20 mM, 22 µA
20000
10 mM, 12 µA
0
-20000 0
1
2
3
4
5
6
7
8
Time (min)
Figure S2.
Page S-3
9
10
11
12
13
14
Absorbance (mAU)
180000
(A)
160000
140000
120000
100000
80000
60000
15 %
40000
10 %
20000
5%
0
-20000 0
2
4
6
8
10
12
14
16
18
20
25000
(B)
20000
15000
10000
5000
0
-5000
0
2
4
6
8
10
12
14
16
18
20
250000
200000
(C)
150000
100000
50000
0
0
-50000
2
4
6
8
10
Time (min)
Figure S3.
Page S-4
12
14
16
18
20
300000
200000
150000
20 kV
17 kV
15 kV
13 kV
10 kV
5 kV
100000
50000
0
0
2
4
6
8
10
12
14
16
18
20
Time (min)
-50000
Figure S4.
200000
Absorbance (mAU)
Absorbance (mAU)
250000
150000
100000
5sec
4sec
3sec
2sec
1 sec
50000
0
0
-50000
5
10
Time (min)
Figure S5.
Page S-5
15
20
Absorbance (mAU)
200000
150000
100000
30 ◦C
25◦C
20 ◦C
50000
0
0
5
10
15
20
Time (min)
-50000
Figure S6.
Absorbance (mAU)
240000
190000
275 nm
260 nm
140000
250 nm
245 nm
90000
240 nm
230 nm
220 nm
40000
210 nm
203 nm
-10000
0
5
10
Time (min)
Figure S7.
Page S-6
15
20
12000
11000
ALS
10000
Absorbance (mAU)
9000
8000
7000
6000
AML
5000
4000
3000
IS
HCZ
2000
1000
0
0
0.5
1
1.5
2
2.5
3
3.5
4
4.5 5 5.5
Time (min)
6
6.5
7
7.5
8
8.5
9
7.5
8
8.5
9
9.5 10
Figure S8.
20000
ALS
18000
Absorbance (mAU)
16000
14000
12000
10000
AML
8000
HCZ
6000
IS
4000
2000
0
0
0.5
1
1.5
2
2.5
3
3.5
4
4.5 5 5.5
Time (min)
Figure S9.
Page S-7
6
6.5
7
9.5 10
Table S1. Performance data for the determination of the studied drugs by the proposed CZE method
AML
HCZ
ALS
1-10
2.5-25
30-300
Intercept (a)
-0.0009
0.1298
0.0846
Slope (b)
0.0110
0.0203
0.0122
Correlation coefficient (r)
0.9999
0.9999
0.9998
S.D. of residuals (Sy/x)
0.0005
0.0026
0.0277
S.D. of intercept (Sa)
0.0004
0.0021
0.0215
S.D. of slope (Sb)
0.0001
0.0002
0.0001
Percentage relative standard deviation, % RSD
0.79
0.67
0.80
Percentage relative error, % Error
0.32
0.27
0.33
Limit of detection, LOD (µg/mL)
0.11
0.33
5.83
Limit of quantitation, LOQ (µg/mL)
0.33
1.01
17.65
Parameter
Linearity range (µg/mL)
Page S-8
Table S2. Robustness data for the determination the studied drugs by the proposed CZE method
Migration times
(min.)
Parameters
AML
ALS
HCZ
AML
ALS
HCZ
4.20
4.40
5.40
0.066
2.976
0.538
5.82
4.33
4.51
5.59
0.065
2.961
0.534
6.21
4.05
4.25
5.15
0.067
2.979
0.538
35
4.10
4.25
5.20
0.064
2.969
0.537
45
4.25
4.80
5.55
0.069
2.994
0.528
15
4.76
4.98
6.13
0.076
2.606
0.524
20
3.46
3.62
4.43
0.076
2.645
0.561
23
4.40
4.65
5.83
0.068
2.805
0.537
27
4.08
4.25
4.95
0.066
2.928
0.585
Standard
Buffer pH
Buffer
Peak area ratios
concocentration
(mM)
Applied voltage
(kV)
Capillary temp.
(oC)
N.B. Each result is the average of three separate determinations.
Page S-9
Table S3. Assay results for the determination of the studied drugs in their synthetic
mixture and reference methods
Ratio
Compound
Amount taken
(g/mL)
Amount found
(g/mL)
% Found
% Found
3.14
3.15
100.29
100.52
7.50
7.50
99.97
99.35
10.00
10.01
100.06
100.24
Mean ± S.D.
100.11± 0.17
100.04± 0.61
% RSD
0.17
% Error
0.10
t
0.22 (2.36)
F
1.68 (19.29)
AML
5.65
5.61
99.26
99.18
13.50
13.71
101.58
100.84
18.00
18.05
100.27
99.71
Mean ± S.D.
100.37± 1.17
99.91± 0.85
% RSD
% Error
1.16
1.0 : 1.8: 23.9 m/m/m
HCZ
AML: HCZ: ALS
Comparison
method
[46]
Proposed method
t
0.67
0.18(2.36)
F
1.62 (5.79)
75.00
73.94
98.59
98.63
179.25
177.94
99.27
101.05
239.00
238.07
99.61
99.82
Mean ± S.D.
99.16± 0.52
99.83± 2.21
% RSD
% Error
0.52
t
0.65(2.36)
F
2.27 (5.79)
ALS
0.30
N.B. Each result is the average of three separate determinations.
The values between parentheses are the tabulated t and F values at P = 0.05 [58].
Page S-10
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