Application of TLC-Spectrodensitometric and Chemometric Methods for Determination of Momenta^® Cream: A Comparative Study Applied on Ternary Mixture

    

    

    Figure 1: The chemical structures of (a) Mometasone Furoate (MF); (b)
Miconazole Nitrate (MIC) and (c) Gentamicin (GM).
    

Experimental

Apparatus and software

• The TLC-spectrodensitometric system: CAMAG TLC scanner 3 S/N 130319 operated with winCATS software, Linomat 5 autosampler (CAMAG, Muttenz, Switzerland), CAMAG microsyringe (100μL). TLC aluminum sheets (20x20 cm) pre-coated with silica gel 60 F₂₅₄ (Merck KgaA, Darmstad, Germany) were used. Calculations were performed using the Excel program.

• Ultraviolet/Visible spectrophotometer (Spectronic Genesys^® with WINPEC^® application software) with1 cm quartz cell, Spectronic, (USA).

• The centrifugation system: Laboratory Centrifuge, Sigma 2-16KL, Sigma 2-16KHL, with order number 10350, 10353.

• Sonicated water bath BranSonic 220, (Zurich, Switzerland).

• All calculations and statistics were carried out on computer using MATLAB^® program version 7.9.

Chemicals and reagents

Pure samples: Standard (MF), (MIC) and (GM) were kindly donated by SIGMA Pharma Co., Quesna, Egypt. Their purity was found to be 100.08±0.39 [2], 100.17±0.13 [36], and 100.02±0.30 [48] according to reported methods, respectively.

Market sample: Momenta^® cream (Jamjoom pharmaceuticals Co., Ltd., Jeddah, Saudi Arabia), labeled to contain 1mg (MF), 20mg (MIC), and 1mg (GENTA) per one gm cream (batch No. TH0101) were purchased from the Egyptian local market.

Solvents: Methanol and chloroform (Analar grade) and formic acid solution was supplied from (Adwic, El Nasr pharmaceutical Chemicals Co., Egypt).

Standard solutions

Stock solutions: Solutions were prepared in methanol of concentrations: 1mgmL^-1 MF, 2mgmL^-1 MIC mL^-1 and in methanol and water of concentration 4mgmL^-1 GM.

Working solutions: Working solutions were freshly prepared by further dilution of suitable volumes from each stock solutions with methanol to get solutions of final concentration for TLCspectrodensitometric method, 0.5mgmL^-1 MF, 1mgmL^-1 MIC, and 2mgmL^-1 GM; for chemometric method, 100μgmL^-1 MF, 200μgmL^-1 MIC, and 2000μgmL^-1 GM.

Procedure

For TLC-densitometric method:

Chromatographic conditions: TLC aluminum sheets 20 x 20 cm pre-coated with 0.25mm silica gel 60 F₂₅₄ were used. The samples were applied as bands (bandwidth: 6mm, bands were spaced 1cm apart from each other and 1.5cm from the bottom edge of the plate). The developing system used was chloroform: methanol: formic acid (4:0.3:0.15, v/v/v) as a mobile phase of total volume approximately 10 milliliters. Linear ascending development was done in a chromatographic tank previously saturated with the developing system for 15min. at room temperature (25±2 °C) to a distance of approximately 8cm from the lower edge (approximately 10min). The developed plates were dried in air for approximately 5min. and scanned at 254nm. The detection was done using Camage TLC scanner 3 operated in the reflectance-absorbance mode. The slit dimension was kept at 3mm x 0.45mm and the scanning speed was 20mm/s. All measurements were performed by winCATS software.

Application to pharmaceutical preparation: A four-gram portion of cream was transferred to a 50mL volumetric flask, taking care to avoid sticking cream to the walls of the volumetric flask. A 30mL portion of methanol and 10mL portion of water was added to the flask, and the cream was allowed to melt by warming at 60^oC in a water bath with constant shaking. The solution was allowed to cool to room temperature. The volume was made up to the mark with methanol and mixed. The solution was centrifuged at 10000rpm for 10min, and a clear supernatant solution was obtained. A portion of the supernatant was diluted with methanol to obtain a final concentration 40μgmL^-1 of MF, 800μgmL^-1 of MIC, and 40μgmL^-1 of GM.

Linearity and construction of calibration curves: Aliquot volumes (1-12 μg band^-1) of MF, (20-45 μg band^-1) of MIC and (1-6 μg band^-1) of GM were separately transferred from their working solutions into 10mL volumetric flasks and diluted to volume with methanol. Aliquot of 10μL of each solution was applied to the TLC plate using a 100μL syringe. The chromatographic conditions were applied and the chromatograms were recorded. The calibration curves were constructed by plotting the recorded peak area versus the corresponding drug concentrations, from which the regression equations were calculated. The calibration curves were made from the average of three experiments.

For chemometric method:

Construction of calibration Set: Multilevel partial factorial design [68] was used for the construction of the calibration and validation sets. A five-level, five-factor calibration design was used. Thirteen mixtures were used for building the calibration model. The laboratory-prepared mixtures of MF, MIC and GM were prepared within their corresponding concentration ranges. The absorption spectra of the prepared mixtures were recorded in the range of 200- 400 nm and transferred to Matlab^® for subsequent data manipulation.

Application to validation set: Into a series of 10mL volumetric flask, accurate aliquots of each component were transferred from their working solutions to prepare twelve mixtures containing different ratios of the cited drugs. The spectra of the prepared solutions from 200 to 400 nm were recorded and transferred to Matlab^®. The concentration of each component was calculated using the constructed model.

Application to pharmaceutical preparation: As described before, then the solution was centrifuged at 10000rpm for 10min, and a clear supernatant solution was obtained. Further dilution was done to obtain a final concentration 40μgmL^-1 of MF, 800μgmL^-1 of MIC, and 40μgmL^-1 of GM.

The concentration of each component was calculated using the constructed PCR and PLS models. When carrying out the standard addition technique, different known concentrations of the pure standard of each drug were added to the pharmaceutical dosage form before proceeding in the previously mentioned procedure.

Results and Discussion

This work was aimed to develop, and validate simple, accurate, selective, and precise analytical approaches which were TLCspectrodensitometric and chemometric methods, for the simultaneous assessment of the ternary mixture of MF, MIC, and GM in their pure form and pharmaceutical dosage form.

TLC-densitometry

This approach offers a simple manner for quantification directly on TLC plate by calculating the optical density of the separated bands. The amounts of compounds are determined by comparing to a standard curve from reference materials chromatographed simultaneously under the same circumstances.

Optimization of the method: To optimize the approach conditions, it was necessary to test the effect of different variables. In order to separate the three drugs from each other’s, several ratios of different developing systems were investigated. Certainly, it was established that the best separation of the cited drugs was achieved by applying the developing system using chloroform: methanol: formic acid (4:0.3:0.15, v/v/v). R_f for MF, MIC, and GENTA were 0.30 ± 0.01, 0.52±0.02, and 0.03±0.01, respectively. Different scanning wavelengths were tried; on using 245 nm where the separated peaks were sharp and symmetrical with minimum noise, as shown in Figure 2.

Figure 2: (A) 2D-TLC chromatogram; (B) 3D-TLC chromatogram of (a) 0.4μg band^-1 of GM, (b) 24μg band^-1 of MF, and (c) 4μg band^-1 of MIC, using chloroform: methanol: formic acid (4:0.3:0.15, v/v/v) as the developing system.

    

    

    Figure 2: (A) 2D-TLC chromatogram; (B) 3D-TLC chromatogram of (a)
0.4μg band-1 of GM, (b) 24μg band-1 of MF, and (c) 4μg band-1 of MIC,
using chloroform: methanol: formic acid (4:0.3:0.15, v/v/v) as the developing
system.
    

Close

Method validation: Method validation was performed according to the International Conference on Harmonization (ICH) guidelines [69] regarding linearity, range, precision, and accuracy, limit of detection and limit of quantitation.

Range and linearity: The linearity of the suggested method was assessed by preparing different calibration curves. Analysis was carried out on a series of standard drug solutions, the calibration curves were constructed between AUC and corresponding concentrations of bands. Linear regression analysis was applied and analytical parameters were calculated. The linear ranges were found to be 1-12 μg band^-1, 20-45 μg band^-1, and 1-6 μg band^-1 for MF, MIC, and GM, respectively. The method at a good linearity and indicated by the values of correlation coefficient. The linear concentration ranges and other statistical parameters for the proposed method were listed in Table 1.

Table 1: Assay parameters and method validation sheet obtained by applying the proposed TLC-spectrodensitometric method for determination of MF, MIC, and GM in ternary mixture.

  

    
Parameter
    
MF
    
MIC
    
GM
  
  

    
Concentration range (μg band-1)
    
1 - 12
    
20 - 45
    
1 - 6
  
  

    
Slope
    
4.7103
    
1.9829
    
5.0829
  
  

    
Standard deviation of the slope (SDb)
    
0.0664
    
0.0201
    
0.0327
  
  

    
Intercept
    
157.7
    
290.39
    
69.76
  
  

    
Standard deviation of the intercept (SDa)
    
0.4764
    
0.6743
    
0.1274
  
  

    
Standard deviation of the residuals (SDy/x)
    
0.5968
    
0.4198
    
0.1368
  
  

    
Number of determinations
    
6
    
6
    
6
  
  

    
Accuracy
    
100.34 ± 1.48
    
100.00 ± 0.34
    
100.29 ± 0.97
  
  

    
Correlation coefficient (r)
    
0.9996
    
0.9998
    
0.9999
  
  

    
Determination coefficient (r2)
    
0.9992
    
0.9996
    
0.9998
  
  

    
Limit of detection, LOD (μg band-1)
    
0.3338
    
1.1222
    
0.0827
  
  

    
Limit of quantitation, LOQ (μg band-1)
    
1.0114
    
3.4006
    
0.2506
  

Table 1: Assay parameters and method validation sheet obtained by applying
the proposed TLC-spectrodensitometric method for determination of MF, MIC,
and GM in ternary mixture.

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Limits of detection and quantitation: The Limit of Detection (LOD) and Limit of Quantitation (LOQ) of the proposed method were calculated, for drugs using a ratio of 3.3 and 10 standard deviations of the blank and the slope of the calibration line, Table 1. The limits of detection were calculated as SD×3.3/slope. Whereas, Limits of quantitation were calculated as SD×10/slope.

Accuracy: For the study of the accuracy of the suggested method, repeated analysis (three times) of different concentrations of MF, MIC, and GM within the linearity range were performed. The accuracy asserted as percentage recoveries and Standard Deviations (SD) (Table 1). By applying standard addition technique to the pharmaceutical formulation, the conflict of excipients was studied. The acceptable accuracy demonstrated that the excipients in the pharmaceutical formulation did not interfere in the analysis of these compounds in the pharmaceutical formulation (Table 2).

Table 2: Application of standard addition technique to the analysis of Momenta^® cream by applying the proposed methods.

  

    
 
    
TLC–densitometry
    
PLS
  
  

    
Taken in μg band-1
    
Found in μg band-1
    
Recovery%*
    
Taken in μg band-1
    
Found in μg band-1
    
Recovery%*
  
  

    
MF
    
5
    
5.02
    
100.35
    
20
    
20.03
    
100.15
  
  

    
MIC
    
25
    
24.88
    
99.5
    
40
    
40
    
100
  
  

    
GM
    
4
    
4
    
100.11
    
30
    
30.01
    
100.03
  
  

    
*Average of three experiments. 
  

Table 2: Application of standard addition technique to the analysis of Momenta® cream by applying the proposed methods.

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Precision: The inter-day and intra-day precision of the proposed method were determined by the analysis of three distinct concentrations of each component, within the linearity range, by three replicate analyses of three pure samples of both drugs on a single day and three ensuing days, for the inter-day and intra-day precisions, respectively. The results expressed as mean percentage recoveries and RSD (Table 3).

Table 3: Application of Intra-day and Inter-day technique to the analysis of MF, MIC, and GM in Momenta^® cream by the proposed TLC–spectrodensitometric method.

  

    

    
Drug
    
Conc. Level (μg mL-1)
    
*% Recovery ± SD
    
%RSD
  
  

    
Inter-day
    
MF
    
5
    
99.67 ± 0.59
    
0.59
  
  

    
7
    
99.85 ± 0.60
    
0.6
  
  

    
9
    
100.67 ± 0.18
    
0.18
  
  

    
MIC
    
25
    
99.74 ± 0.54
    
0.54
  
  

    
30
    
100.58 ± 0.22
    
0.22
  
  

    
35
    
99.55 ± 0.30
    
0.3
  
  

    
GM
    
3
    
99.32 ± 1.19
    
1.2
  
  

    
4
    
100.13 ± 0.41
    
0.41
  
  

    
5
    
99.87 ± 0.59
    
0.59
  
  

    
Intra-day
    
MF
    
5
    
99.69 ± 0.55
    
0.55
  
  

    
7
    
100.32 ± 0.31
    
0.31
  
  

    
9
    
99.93 ± 0.39
    
0.39
  
  

    
MIC
    
25
    
99.55 ± 0.68
    
0.68
  
  

    
30
    
100.18 ± 0.26
    
0.26
  
  

    
35
    
99.71 ± 0.54
    
0.54
  
  

    
GM
    
3
    
100.45 ± 0.40
    
0.4
  
  

    
4
    
99.53 ± 0.49
    
0.49
  
  

    
5
    
100.08 ± 0.31
    
0.31
  
  

    
*Average of three experiments. 
  

Table 3: Application of Intra-day and Inter-day technique to the analysis of MF,
MIC, and GM in Momenta® cream by the proposed TLC–spectrodensitometric
method.

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Selectivity: Selectivity was confirmed by analyzing different mixtures containing drugs in different ratios within the linearity range. Satisfactory results were shown in Table 4. The conflict of excipients in the pharmaceutical formulations were studied by applying standard addition method to the pharmaceutical formulation Table 2; which did not interfere in the analysis of these compounds in the pharmaceutical formulation.

Table 4: Determination of MF, MIC, and GM in laboratory prepared mixtures by the proposed TLC-spectrodensitometric method.

  

    

    
Mix ratio
    
MF
    
MIC
    
GM
  
  

    
1
    
1:10:02
    
99.75 ± 0.57
    
100.54 ± 1.20
    
99.90 ± 0.98
  
  

    
2
    
1:04:01
    
99.75 ± 0.69
    
99.97 ± 0.98
    
100.09 ± 1.05
  
  

    
3
    
2:05:01
    
99.00 ± 1.05
    
99.95 ± 0.95
    
99.59 ± 0.79
  
  

    
4
    
1:20:1*
    
99.51 ± 0.77
    
100.59 ± 0.95
    
99.90 ± 1.05
  
  

    
5
    
3:05:01
    
100.54 ± 0.77
    
99.89 ± 0.89
    
99.00 ± 0.99
  
  

    
*Ratio in Momenta® cream. 
  

Table 4: Determination of MF, MIC, and GM in laboratory prepared mixtures by
the proposed TLC-spectrodensitometric method.

Close

System suitability: System suitability was checked by calculating different parameters (Table 5). The obtained values were in the acceptable ranges when compared to the reference values [70].

Table 5: System suitability parameters of the proposed TLC-spectrodensitometric method of MF, MIC and GM in Momenta^® cream.

  

    
Parameter
    
MF
    
MIC
    
GM
    
Reference value
  
  

    
Rf value
    
0.30 ± 0.01
    
0.52 ± 0.02
    
0.03 ± 0.01
    

  
  

    
T (tailing factor)
    
0.91
    
0.9
    
0.87
    
T= 1.15 - 0.95 & T = 1 for symmetric peak
  
  

    
Rs (experimental resolution)
    
2.66
    
3.42
    
1.72
    
Rs >1.5
  

Table 5: System suitability parameters of the proposed TLC-spectrodensitometric
method of MF, MIC and GM in Momenta® cream.

Close

Chemometric method

Among the different regression methods existing for multivariate calibration, the factor analysis based on Principal Component Regression Model (PCR) and Partial Least Squares (PLS) regression have received considerable attention in the chemometrics literature [71]. PCR predates PLS. In cases where only partial knowledge of components is present, PCR and PLS can work well. PCR assumes that error is only in the instrumental response and concentration matrix is error-free, while PLS assumes that error is equally distributed between concentration matrix and instrumental response (spectral) matrix. Thus, PLS produces more robust model as it removes noise from both absorbance and concentration data [72].

The calibration set was constructed using the absorption spectra set of 15 mixtures, as listed in Table 6. The initial models were found to give bad results, so the regions below 205 and above 300nm were rejected. Cross-validation methods leaving out one sample at a time was employed. The Root Mean Squares Error of Cross-Validation (RMSECV) was calculated which is used as a diagnostic test for examining the errors in the predicted concentrations. It indicated both precision and accuracy of predictions. The selected model was that with the smallest number of factors such that RMSECV for that model was not significantly greater than RMSECV from the model with additional factor. Four factors were found to be optimum for the mixture, as shown in Figure 3 for PCR and PLS.

Figure 3: RMSECV of the calibration set of MF, MIC, and GM as a function of latent variables of (a) PCR and (b) PLS models.

    

    

    Figure 3: RMSECV of the calibration set of MF, MIC, and GM as a function of latent variables of (a) PCR and (b) PLS models.
    

Close

Table 6: Concentration of MF, MIC, and GM in the calibration set using PCR and PLS models.

  

    
Experimental No.
    
Concentration (μg mL-1)
  
  

    
MF
    
MIC
    
GM
  
  

    
1
    
6
    
12
    
6
  
  

    
2
    
10
    
10
    
4
  
  

    
3
    
4
    
14
    
10
  
  

    
4
    
6
    
14
    
4
  
  

    
5
    
4
    
12
    
4
  
  

    
6
    
8
    
11
    
10
  
  

    
7
    
10
    
13
    
8
  
  

    
8
    
6
    
13
    
10
  
  

    
9
    
10
    
12
    
10
  
  

    
10
    
2
    
14
    
8
  
  

    
11
    
8
    
10
    
2
  
  

    
12
    
6
    
10
    
8
  
  

    
13
    
8
    
12
    
8
  
  

    
14
    
4
    
13
    
2
  
  

    
15
    
4
    
10
    
6
  

Table 6: Concentration of MF, MIC, and GM in the calibration set using PCR and
PLS models.

Close

Model validation: To assess the prediction ability of the suggested models, an external validation set of 12 mixtures was used as listed in Table 6. The predicted concentrations were compared with the true concentrations of each component in each sample. The Root Mean Squared Errors of Prediction (RMSEP) and the regression equations for the predicted versus actual concentration are listed in Table 7 as diagnostic tools for model validation. The results indicated the higher predictive ability of the PLS model than that of PCR model to analyze the laboratory-prepared mixtures (validation set) within the accepted range, as shown in Table 7, where PCR was unable to interpret this complex model, as it might require a larger number of samples for accurate calibration. The proposed model was also applied for the determination of Momenta^® cream, and the validity of the proposed procedures was further assessed by applying the standard addition technique showing no excipients interference. The results obtained are shown in Table 2.

Table 7: Summary of results obtained by applying the diagnostic tools for model validation of the PCR and PLS models with MF, MIC, and GM.

  

    
Validation parameters
    
PCR
    
PLS
  
  

    
MF
    
MIC
    
GM
    
MF
    
MIC
    
GM
  
  

    
Slope
    
0.9997
    
1.0541
    
0.9701
    
0.9351
    
0.9054
    
1.0451
  
  

    
Intercept
    
0.2534
    
0.0981
    
0.1535
    
0.1234
    
0.2157
    
0.7311
  
  

    
Correlation coefficient (r)
    
0.9999
    
0.9996
    
0.9997
    
0.9995
    
0.9999
    
0.9999
  
  

    
RMSEP
    
0.259
    
0.095
    
0.141
    
0.053
    
0.155
    
0.094
  

Table 7: Summary of results obtained by applying the diagnostic tools for model
validation of the PCR and PLS models with MF, MIC, and GM.

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Statistical analysis

Table 8 showed statistical comparison of the results obtained by the proposed methods and reported methods for MF [7], MIC [36], and GM [48] for TLC-spectrodensitometric method, and official method {-} for chemometric method. The calculated t and F values were less than the theoretical ones indicating that there was no significant difference between the proposed and the official methods with respect to accuracy and precision.

Table 8: Statistical comparison between the results obtained by the proposed TLC-spectrodensitometric method and the reported methods for the determination of MF, MIC and GM in pure powder form.

  

    
Parameter
    
MF
    
MIC
    
GM
  
  

    
Reported Method
    
TLC
    
PLS
    
Reported Method
    
TLC
    
PLS
    
Reported Method
    
TLC
    
PLS
  
  

    
Mean
    
100.1
    
100.34
    
-
    
100.17
    
100
    
-
    
100.02
    
100.29
    
-
  
  

    
Standard Deviation (SD)
    
1.039
    
1.48
    
-
    
0.13
    
0.34
    
-
    
0.3
    
0.97
    
-
  
  

    
N
    
7
    
0
    
-
    
3
    
6
    
-
    
3
    
6
    
-
  
  

    
Variance
    
1.08
    
2.19
    
-
    
0.0169
    
0.1156
    
-
    
0.09
    
0.94
    
-
  
  

    
Student, t
    
 
    
0.33

      (2.228)
    
-
    
 
    
1.08

      (2.306)
    
-
    
 
    
0.62

      (2.306)
    
-
  
  

    
F
    
 
    
2.03

      (4.39)
    
-
    
 
    
6.84

      (19.3)
    
-
    
 
    
10.44

      (19.3)
    
-
  

Table 8: Statistical comparison between the results obtained by the proposed TLC-spectrodensitometric method and the reported methods for the determination of
MF, MIC and GM in pure powder form.

Close

Conclusion

This work presented a comparative study on two analytical techniques based on UV spectrophotometry which were TLCdensitometric method and chemometric-assisted spectrophotometric method (PLS) and (PCR). Both techniques were successfully applied for the simultaneous estimation of the ternary mixture of MF, MIC, and GM in their pure form and topical pharmaceutical formulation. The TLC-densitometric method has the advantage over HPLC methods as it minimizes the usage of reagents which supports the ecofriendly behavior of green chemistry, it minimizes the time required for analysis, and it utilizes the merit of applying several sample bands on TLC plate, which may be more advantageous for regulatory quality control laboratories. In addition, the method is inexpensive and does not require certain types of stationary phases, but still, the method fulfills the same validation parameters and efficiency when compared to reported HPLC method. Meanwhile, the chemometric method has the advantage of being simpler as it does not require special reagents or chemicals, and it is considered to be time- and cost-saving, but it requires a special software (Matlab). It was found that PLS preceded PCR in the analysis of such complex mixtures. As a final conclusion, the results obtained by the two proposed methods were reliable, accurate, and precise. Hence, both methods can be employed for routine quality control analysis as alternative methods to different HPLC techniques in quality control laboratories lacking the required facilities for those expensive techniques.

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Citation: Salem H, Omar MA, Derayea SM and Khalil AA. Application of TLC-Spectrodensitometric and Chemometric Methods for Determination of Momenta® Cream: A Comparative Study Applied on Ternary Mixture. Austin J Anal Pharm Chem. 2021; 8(1): 1131.

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