Received: 11 August 2018
Accepted: 23 September 2018
DOI: 10.1002/bio.3568
RESEARCH ARTICLE
Validated spectroscopic methods for the estimation of triamterene in bulk powder and capsule form via derivatization reactions Fawzia A. Ibrahim1 | Manal M. Fouad2,3 Ebtesam S. Mahmoud3
|
Noha S. Rashed3
|
Mona E. Fathy1
|
1
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, University of Mansoura, Mansoura, Egypt
2
Department of Analytical Chemistry, Faculty of Pharmacy, October University for Modern Sciences and Arts, Cairo, Egypt
3
Department of Analytical Chemistry, Faculty of Pharmacy, Al‐Azhar University, Cairo, Egypt Correspondence Mona E. Fathy, Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, University of Mansoura, 35516, Mansoura, Egypt. Email:
[email protected]
Abstract Sensitive, simple and specific spectrophotometric and spectrofluorimetric methods were developed for the determination of triamterene in bulk powder and pharmaceutical dosage form. The spectrophotometric method (Method A) is based on the formation of an ion‐pair complex with eosin Y in acetate buffered solution of pH 3.7 followed by measuring the absorbance at 545 nm. The absorbance–concentration plot is rectilinear over the range 3.0–15.0 μg/mL with a limit of detection (LOD) of 0.429 μg/mL and a limit of quantitation (LOQ) of 1.031 μg/mL. The spectrofluorimetric method (Method B) is based on the reaction of triamterene with 7‐ chloro‐4‐nitrobenzo‐2‐oxa‐1,3‐diazole (NBD‐Cl) in basic solution (pH 10) to form a product with high fluorescence measured at 546 nm after being excited at 438 nm. The plot of fluorescence versus concentration is linear within the range 2.0–10.0 μg/mL. The suggested methods were applied for the analysis of commercial capsules containing the studied drug with successful results. The results obtained from the proposed method were statistically compared with those of a reported one and revealed good agreement. The presented methods are useful in routine analysis of triamterene in laboratories of quality control. KEY W ORDS
capsules, Eosin Y, NBD‐Cl, spectrofluorimetry, spectrophotometry, triamterene
1
|
I N T RO D U CT I O N
determination of TRM based on its reaction with eosin Y and 7‐
Triamterene (TRM); is chemically designated as 2,4,7‐triamino‐6‐ phenylpteridine[1] (Figure 1). It is a diuretic with mild action. It belongs to the potassium‐sparing family that acts directly to decrease potassium ion release and to prevent the re‐absorption of chloride ions.[2]
chloro‐4‐nitrobenzo‐2‐oxa‐1,3‐diazole
(NBD‐Cl).
The
suggested
methods were validated perfectly according to guidelines of ICH,[20] and applied for the determination of the studied drug in its capsules with successful results.
Several methods have been reported for the assay of TRM. Surveying the literature showed that several methods of analysis of TRM either
2
EXPERIMENTAL
|
alone or simultaneously with other drugs were published including spectrophotometric methods,[3–8] spectrofluorimetric,[9] high‐performance liquid chromatography (HPLC)[8,10–18] and thin‐layer chroma[7,19]
tography (TLC)
Luminescence. 2018;1–9.
and
spectrofluorimetric
|
Instrumentation
• Shimadzu, UV‐vis 1601PC spectrophotometer (Tokyo, Japan),
methods.
The present study aimed to introduce accurate and precise spectrophotometric
2.1
methods
for
the
connected with UV probe program with two matched 1 cm pathlength quartz cell.
wileyonlinelibrary.com/journal/bio
© 2018 John Wiley & Sons, Ltd.
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the same solvent to get TRM working standard solutions of 100 μg/ mL concentration.
2.5 FIGURE 1
Structural formulae of triamterene
Construction of the calibration curves
|
2.5.1
Method A
|
Aliquots of drug standard solution of (100.0 μg/mL) containing (30.0– • Spectrofluorimeter (Shimadzu, Model RF 1501) supplied with lamp of xenon and 1‐cm cells made of quartz. • Measurements of pH were performed with Jenway 3150 pH meter (Jenway, Stone, UK).
150.0 μg) were transferred quantitatively into a number of 10 mL measuring flasks; the volumes were diluted to 6 mL with water. Then, 1.2 mL was taken from 2 × 10−3 M eosin Y solution and added to the flasks with mixing before adding 1.5 mL of acetate buffer of pH 3.7. The mixture was adjusted to the mark with distilled water then the absorption intensity was measured at a wavelength of 545 nm against an appropriate blank prepared simultaneously. The calibration curve
2.2
Samples
|
2.2.1
Pure sample
|
Pharmaceutical grade TRM was kindly supplied by EIPICO (10th of Ramadan City, Egypt).
2.2.2
Market sample
|
was obtained by plotting the measured absorption intensity versus TRM concentration in micrograms per milliliter (μg/mL). Then, the equation of regression was derived.
2.5.2
Method B
|
Into a series of 20 mL test tubes, aliquots of working standard TRM solution (100 μg/mL) equivalent to (20.0–100.0 μg) of TRM were
Dyrenium® capsules; lot no 702d, labeled to contain 50 mg TRM
transferred. Then, 1.0 mL of NBD‐Cl solution (0.1%) and 1.2 mL borate
(Wellspring Pharmaceutical, Canada).
buffer (pH 10.0) were added to each tube and mixed well. The test tubes were heated in a water bath at 80°C for 25 min and then cooled.
2.3
|
Chemicals and reagents
Next, 0.2 mL of concentrated hydrochloric acid (HCl) was added to each tube and mixed well. The contents of the test tubes were
All reagents were of analysis grade and solvents used were of spectroscopy grade, distilled water was used during the work. • Eosin Y (2,4,5,7‐tetrabromofluorescein) (Sigma‐Aldrich, Hamburg, Germany); 2 × 10−3 M aqueous solution prepared in distilled water. • Acetate buffers (0.2 M, pH 3–5) were prepared by adding 0.2 M
transferred quantitatively into a number of 10 mL measuring flasks and the volumes were adjusted to the marks with methanol. The fluorescence intensities of the solutions were measured at 438 and 546 nm as excitation and emission wavelengths, respectively. The calibration curve was obtained by plotting the relative fluorescence intensity of TRM against the final TRM concentration (in μg/mL). Then, the equation of regression was deduced.
sodium acetate solution to 0.2 M acetic acid solution to get appropriate pH values. • NBD‐Cl (Sigma‐Aldrich). A solution of 0.1% NBD‐Cl was prepared daily in methanol.
2.6
|
Analysis of TRM in raw material
The described methods were used to determine the purity of TRM in its raw material applying the steps detailed in the section of
• Borate buffer solutions (0.1 M, pH 7.5–11.5) were prepared by
“Construction of the Calibration Curves” for both methods (A and B).
mixing appropriate volumes of 0.1 M sodium hydroxide (NaOH)
The percentages found were then calculated from the regression
and 0.1 M boric acid.
equations.
• Boric acid (Gomhouria Co., Alexandria, Egypt), 0.1 M solution was prepared by heating boric acid in distilled water. • NaOH (Gomhouria Co, Alexandria, Egypt), 0.1 M solution was prepared in distilled water. • HCl, methanol (Sigma‐ Aldrich, Riedel‐de Haen and EL Nasr Co.).
2.7
|
Reaction stoichiometry for Methods A and B
The reaction stoichiometry between TRM and both reagents; eosin Y and NBD‐Cl was determined by applying Job's method[21] of continuous variation. This was performed using concentrations of the reagents and drug solutions of the same molarity; 1 × 10−4 M for Method A and 1 × 10−3 M for Method B and where different volumes
2.4
|
Standard solutions
TRM powder (100.0 mg) was accurately weighed and transferred into 100 mL measuring flask, then dissolved in the least amount of metha-
of the drug and reagent were used to obtain different ratios.
2.8
|
Procedure for commercial capsules
nol, the flask was filled to the mark with distilled water (Method A) or
The contents of ten capsules (Dyrenium®) were mixed perfectly. An
methanol (Method B) to obtain stock solutions of 1.0 mg/mL TRM.
accurate quantity of the mixed contents (equivalent to about
Each of the prepared solutions was then diluted appropriately using
100 mg of TRM) was quantitatively transferred into a 100 mL
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measuring flask and dissolved in 5 mL of methanol with the aid of
The proposed method is based on ion pair formation between
ultra‐sonication for 15 min. The content in the volumetric flask was
TRM and eosin Y. This complex was formed when the basic center
filled to the mark with water (Method A) or with methanol (Method
in the drug (NH2 group) interacts electrostatically with COO– ion of
B), mixed well and then filtered. This stock solution (1 mg/mL) was
eosin in an acidic medium. This interaction increases the delocalization
diluted stepwise using the same solvent to get the wanted
of eosin electrons resulting in a shift of the maximum absorption
concentrations.
wavelength of eosin of about 30 nm. Maximum absorbance of the
The obtained solutions were analyzed according to the steps
formed complex was found to be 545 nm (Figure 2, Scheme 1). This
detailed in the section of “Construction of Calibration Curve” and then
reaction was used to construct a novel spectroscopic method for the
the drug concentrations were calculated from previously derived
assay of TRM.
regression equations.
3.2 3
RESULTS AND DISCUSSION
|
Spectrofluorimetric Method B
|
NBD‐Cl reagent forms chromogenic and fluorescent products with primary or secondary amines. Since TRM contains NH2 groups, it
In this work, a spectrophotometric method using eosin Y and a
reacts with NBD‐Cl in basic medium as shown in Figure 2. Under
spectrofluorimetric method using NBD‐Cl were utilized as useful tools
the developed experimental conditions, the maximum fluorescence
for accurate determination of TRM in pure form in addition to its phar-
intensity was determined at 546 nm while excitation took place at
maceutical dosage form.
438 nm (Figure 3, Scheme 2. It was necessary before measuring the fluorescence intensity of the reaction mixture to add concentrated HCl. This prior step of acidification decreased slowly the fluorescence
3.1
|
Spectrophotometric Method A
of NBD‐OH resulting from the hydrolysis of NBD‐Cl.
Formation of ion‐pair complexes between eosin Y and compounds with basic nature have been frequently used in the analysis of many pharmaceutical drugs, spectrophotometrically. Because of the insolubility of the formed complexes in water, it was often extracted into organic solvent or solubilized by the aid of a non‐ionic surfactant such as carboxymethylcellulose. In this study, the complex solubility was elevated by applying a certain procedure. This procedure which was mentioned under “Construction of the Calibration Curves” depended
3.3
Optimization of the reactions conditions
|
All factors that affected the reaction of TRM with eosin (Method A) or NBD‐Cl (Method B) have been investigated as illustrated in the following sections.
3.3.1
|
Effect of pH
on adding eosin Y solution to a highly diluted drug solution at neutral
Method A
pH and mixing well before adding acetate buffer.
The pH effect on the absorption intensity of the formed ion pair of TRM with eosin Y was studied within the pH range 3.0–5.0. It was
FIGURE 2 Absorption spectra of eosin Y (2 × 10−3 M) in water ( )ــand RX (eosin Y reaction product with TRM) (6.0 μg/mL) in water at pH 3.7 (_._._._)
SCHEME 1 Suggested reaction mechanism of TRM with eosin‐Y
FIGURE 3 Fluorescence spectra of the reaction product of TRM (6.0 μg/mL) with NBD‐Cl at pH 10.0 at λex 438 nm ( )ــand λem 546 nm (......)
4
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the absorbance intensity. It was found that 1.5 mL of 0.2 M buffer solution was sufficient to give maximum absorbance value, as shown in Figure 6.
Method B The influence of the volume of borate buffer on the values of fluorescence intensity of the resultant product was studied. This was performed by taking different volumes (0.2–2 mL) of 0.1 M borate buffer of pH 10.0. Figure 7 shows that the highest value of fluorescence intensity was attained using 1.2 mL of 0.1 M borate buffer
SCHEME 2
Suggested reaction mechanism of TRM with NBD‐Cl
found that by elevating pH values, the absorbance values increased subsequently till pH 4.0. After which a slight decrease in absorbance was achieved. So, acetate buffer solution of pH 3.7 ± 0.2 was selected as the optimum pH value throughout the spectrophotometric study
3.3.3
|
Effect of volume of reagent
Method A The influence of the volume of eosin Y was studied using different volumes (0.2 to 2.0 mL) of eosin Y (2 × 10−3 M). It was found that 1.2 mL of the dye solution was sufficient to give maximum absorbance, as shown in Figure 8.
(Figure 4).
Method B The pH effect on the fluorescence intensity of the reaction product of TRM with NBD‐Cl was investigated within the range pH 7.5–11.5. Optimum fluorescence intensity was achieved at pH 10 ± 0.2 (Figure 5).
3.3.2
|
Effect of buffer volume
Method A Different volumes (0.5–4.5 mL) of acetate buffer solution (0.2 M) of
FIGURE 6 Effect of volume of 0.2 M acetate buffer pH 3.7 on the absorbance of the reaction product of TRM with eosin Y (2 × 10−3 M)
pH 3.7 were used to study the effect of acetate buffer volume on
FIGURE 4 Effect of pH of 0.2 M acetate buffer on the absorbance of the reaction product of TRM with eosin Y (2 × 10−3 M)
FIGURE 7 Effect of different volumes of 0.1 M borate buffer pH 10.0 on the fluorescence intensity of the reaction product of NBD‐Cl and (6.0 μg/mL) TRM at 546 nm (λex 438 nm)
FIGURE 5 Effect of pH of 0.1 M borate buffer on the fluorescence intensity of the reaction product of (6.0 μg/mL) TRM with 0.1% NBD‐Cl at 546 nm (λex 438 nm)
FIGURE 8 Effect of volume of eosin Y (2 × 10−3 M) on the absorbance of the reaction product of TRM with eosin Y
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Method B
3.4
The effect of NBD‐Cl volume on the fluorescence intensity of the formed product was investigated utilizing increasing volumes of 0.1% NBD‐Cl solution. It was found that the fluorescence intensity of the reaction product increased proportionally with increasing the volume of the reagent up to 0.8 mL and remained constant till
|
Reaction stoichiometry
From Job's method of continuous variation; it was concluded that the reaction between TRM and eosin Y or between TRM and NBD‐Cl proceeds in a ratio of 1:1 which confirmed that one molecule of TRM reacts with one molecule of eosin Y or NBD‐Cl (Figures 12, 13).
1.5 mL. Further increase in the volume of reagent, the fluorescence intensity deceased gradually. Hence, 1 mL of NBD‐Cl solution (0.1%) was selected as an optimal volume for maximal fluorescence intensity (Figure 9).
3.3.4
|
Effect of time and temperature
Method A The complex was formed instantaneously within a few seconds and was stable for at least seven hours. The reaction with eosin Y was performed at room temperature. Increasing temperature of the reaction mixture resulted in the formation of a precipitate.
FIGURE 11 Effect of heating time on the fluorescence intensity of the reaction product of (6.0 μg/mL) TRM with NBD‐Cl at 546 nm (λex 438 nm)
Method B Effect of temperature was investigated by heating the reaction mixture at different temperatures (30–100°C) with constant heating time. Also, the effect of heating time was studied by heating the reaction mixture for different time intervals (5–40 min). Obtained results ascertained that the reaction was temperature dependent, and the highest fluorescence intensity was achieved by heating the reaction mixture at 80 ± 2°C for 25 ± 2 min (Figures 10, 11).
FIGURE 12 Stoichiometry of the reaction of TRM (1 × 10−4 M) with eosin Y (1 × 10−4 M) by continuous variation method.
FIGURE 9 Effect of different volumes of 0.1% NBD‐Cl on the fluorescence intensity of its reaction product with TRM (6.0 μg/mL) at 546 nm (λex 438 nm)
FIGURE 10 Effect of heating temperature on the fluorescence intensity of the reaction product of (6.0 μg/mL) TRM with NBD‐Cl at λem 546 nm (λex 438 nm)
FIGURE 13 Stoichiometry of the reaction of TRM (1 × 10−3M) and NBD‐Cl (1 × 10−3M) solutions by continuous variation method
FIGURE 14 Calibration curve of the reaction product of TRM with eosin Y at λmax 545 nm
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ET AL.
4 | V A L I D A T I O N OF T H E P R O P O S E D METHODS 4.1
|
Linearity and range
Under the optimal conditions detailed earlier, calibration graphs were obtained by plotting the absorption intensity of the formed eosin Y–TRM complex versus the concentration of the drug in μg/mL (Method A) and fluorescence intensity of the yellow colored product FIGURE 15 Calibration curve of the reaction product of TRM with 0.1% NBD‐Cl at λem 546 nm (λex 438 nm)
with NBD‐Cl against corresponding TRM concentration in μg/mL (Method B) (Figures 14, 15). The ranges of concentration obtained were 3.0–15.0 μg/mL for Method A and 2.0–10.0 μg/mL for Method B as illustrated in Table 1. Linear regression equations were as follow:
TABLE 1 Analytical performance data for the determination of TRM by the proposed methods Eosin Y method
NBD‐CL method
Parameter
Method A
Method B
Linearity range (μg/mL)
3.0–15.0
Intercept (a)
0.3336
32.81
Slope (b)
0.0785
21.82
Correlation coefficient (r)
0.9997
0.9997
Standard deviation of residuals (Sy/x)
0.0097
1.523
Standard deviation of intercept (Sa)
1.048
1.595
Standard deviation of slope (Sb)
9.486
0.241
Percentage relative standard deviation, %RSD
1.821
1.844
Percentage relative error, %Error
0.812
0.822
Limit of detection, LOD (μg/mL)
0.429
0.241
Limit of quantitation, LOQ (μg/mL)
1.031
0.371
A ¼ 0:3336 þ 0:0785 C ðr ¼ 0:9997Þ ðMethod AÞ FI ¼ 32:81 þ 21:82 C ðr ¼ 0:9997Þ ðMethod BÞ where A is the absorbance of the TRM–eosin Y complex, FI is the
TABLE 2 methods
2.0–10.0
fluorescence intensity of TRM–NBD‐Cl colored product, C is TRM concentration in μg/mL and r is the coefficient of correlation. By analyzing the data statistically,[22] good statistic values were obtained as shown in Table 1. These good values verified the calibration curves linearity.
4.2
|
Detection and quantitation limits
The limit of detection (LOD) and limit of quantitation (LOQ) limits were calculated according to the guidelines of ICH[20] using the equations: 3.3 Sa/b and 10 Sa/b, respectively, where Sa is the standard deviation of the intercept and b is the slope of the calibration curve.
Assay results for the determination of the TRM in pure form by the proposed spectrophotometric, spectrofluorimetric and comparison Proposed method
Compound TRM Method A
Amount taken (μg/mL)
Amount found (μg/mL)
% Found
3.0
2.902
96.73
101.07
6.0 9.0 12.0 15.0
6.043 9.088 12.105 14.874
100.72 100.98 100.88 99.16
100.48 99.69
99.69
100.41
Mean ± standard deviation
1.821
t‐Test
0.634 (2.446)
F ‐Test
7.043 (19.246)
TRM Method B
Comparison method6 % Found
0.692
2.0
1.933
96.67
100.36
4.0 6.0 8.0 10.0
4.055 6.025 8.05 9.937
101.39 100.43 100.61 99.37
101.29 100.58
99.69
100.74
Mean ± standard deviation
1.838
t‐Test
0.941 (2.446)
F ‐Test Note: Each result is the average of three separate determinations. The figures between parentheses are the tabulated t and F values at P = 0.05.[22]
14.293 (19.246)
0.486
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LOQ and LOD values for TRM by the developed spectrophotometric
Statistical analysis of the proposed data using Student's t‐test and var-
and spectrofluorimetric methods are given in Table 1.
iance ratio F ‐ test[22] revealed no appreciable difference between both the proposed and comparison methods regarding accuracy and
4.3
|
precision, respectively (Table 2).
Accuracy and precision
The comparison method[6] involves zero‐order spectrophotomet-
The accuracy of the developed method was proved by comparing the
ric method where TRM solution was scanned in the range from 200
results of the proposed spectrophotometric or spectrofluorimetric
to 400 nm and the peaks were observed at a maximum wavelength
method with the data obtained from the comparison method.[6]
(λmax) of 363 nm.
TABLE 3
Precision data for the determination of TRM by the proposed spectrophotometric and spectrofluorimetric methods Method A TRM concentration (μg/mL)
Parameters Intra‐day
%Found (−x) ± SD %RSD %Error
Inter‐day
%Found (−x) ± SD %RSD %Error
Method B TRM concentration (μg/mL)
3.0
9.0
15.0
4.0
6.0
100.30 100.98 101.36 100.88 ± 0.537 0.532 0.244
102.07 98.91 100.88 100.62 ± 1.596 1.586 0.421
101.10 101.86 98.80 100.58 ± 1.593 1.584 0.419
2.0 99.47 99.24 99.96 99.56 ± 0.368 0.370 0.202
98.26 100.46 101.73 100.15 ± 1.756 1.753 0.442
101.48 100.28 97.84 99.87 ± 1.859 1.816 0.449
101.23 99.53 101.66 100.81 ± 1.126 1.117 0.353
100.16 101.7 99.86 100.57 ± 0.987 0.981 0.331
101.15 98.04 101.675 100.28 ± 1.964 1.958 0.467
101.25 101.46 99.05 100.59 ± 1.335 1.327 0.385
99.31 101.82 100.76 100.63 ± 1.26 1.252 0.372
98.57 99.67 102.11 100.12 ± 1.812 1.810 0.448
Note: SD, standard deviation; %RSD, percentage relative standard deviation; %Error, percentage relative error.
TABLE 4
Robustness of the proposed methods using TRM (15.0 μg/mL) (Method A) and (6.0 μg/mL) (Method B) Method A
Parameter
Amount found (μg/mL)
Method B %Found
Reagent volume
Parameter
Amount found (μg/mL)
%Found
Reagent volume
1.0
14.998
99.99
1.2
15.215
101.43
1.4
14.629
97.53
(−x)
0.8
5.871
97.89
1
5.981
99.68
1.2
5.942
99.04
99.65
98.87
±SD
1.972
0.907
%RSD
1.978
0.917
%Error
0.468
pH
0.317 pH
3.5
14.82
98.80
9.8
5.932
98.93
3.7
14.87
99.14
10
6.092
101.53
3.9
14.72
98.12
10.2
5.983
98.68
(−x)
(−x)
99.71 100.06
±SD
0.519
±S.D.
1.334
%RSD
0.526
%RSD
1.333
%Error
0.240
%error
0.384
Buffer volume
Buffer volume
1
14.71
98.04
1
5.93
98.39
1.5
14.89
99.31
1.2
5.985
99.76
2
14.74
98.29
1.4
5.870
97.88
98.54
(−x)
(−x)
98.67
±SD
0.672
±S.D.
0.972
%RSD
0.681
%RSD
0.985
%Error
0.273
%error
0.328
Note: Each result is the average of three separate determinations. SD, standard deviation; %RSD, percentage relative standard deviation; %Error, percentage relative error.
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TABLE 5 Assay results for the determination of the TRM in its pharmaceutical dosage form by the proposed spectrophotometric and spectrofluorimetric methods Proposed method Compound Method A Dyrenium 50 mg
Amount taken (μg/mL)
Amount found (μg/mL)
%Found
Comparison method6 %Found
3.0
2.901
96.73
99.34
6.0 8.0 12.0 15.0
6.043 8.078 12.105 14.874
100.72 100.98 100.88 99.16
101.76 102.21 98.37 99.64
99.69
100.26
Mean ± standard deviation
1.815
t‐Test
0.519 (2.306)
F ‐Test
1.647
1.214 (6.388)
Method B Dyrenium 50 mg
2.0
96.67
96.67
99.34
4.0 5.0 8.0 10.0
101.39 100.43 316.30 401.60
101.39 100.43 100.61 99.37
101.76 102.21 98.37 99.64
99.69
100.26
Mean ± standard deviation
1.838
t‐Test
0.516 (2.306)
F ‐Test
1.240 (6.388)
1.647
Note: Each result is the average of three separate determinations. The figures between parentheses are the tabulated t and F values at P = 0.05.[22]
4.3.1
|
Intra‐day precision
The obtained results were compared statistically with a comparison
Replicate analysis of three concentrations of TRM was performed on
method[6] by applying F ‐test and student's t‐test at the 95%
three consecutive times in the same day to assess intra‐day precision
confidence level[22] (Table 5).
as shown in Table 3.
6 4.3.2
|
|
CO NC LUSIO N
Inter‐day precision
Replicate analysis of three concentrations of TRM was carried out on
In this work, accurate, sensitive, reproducible and inexpensive spectro-
three consecutive days to assess inter‐day precision as shown in
scopic methods were constructed to study the selective quantitation
Table 3.
of TRM in its bulk powder and pharmaceutical preparation. The validity of both methods has been proven by the good results obtained.
4.4
|
Method robustness
The proposed methods do not need expensive or complex instruments. They are rapid and simple and free from any interference.
Small changes to the parameters of the method such as reagent volume,
Moreover, the employed reagents are available in laboratories of
buffer pH, and buffer volume were investigated in order to evaluate the
analysis. They are cheap with perfect shelf‐life. Hence, the developed
robustness of the proposed methods. These changes that might take
methods can mainly be used in routine testing of quality control
place during the experimental operation did not greatly affect the
of TRM.
measured responses. The results are summarized in Table 4. ORCID
4.5
|
Selectivity
The selectivity of the developed methods was investigated by noticing any interference found from common capsules excipients such as magnesium stearate, lactose, sodium lauryl sulfate and gelatin. It was observed that these substances did not interfere with the proposed methods results.
5
|
A P P L I C A T I O N TO C A P S U L E S
Mona E. Fathy
http://orcid.org/0000-0001-5247-9779
RE FE RE NC ES [1] J. M. O’Niel, P. E. Heckelman, B. K. Cheri, J. K. Roman, M. C. Kenny, R. Maryann, D. Arecca, The Merck Index (an encyclopedia of chemicals, drugs and biologicals), 14th ed., Merck Research Laboratories, San Francisco, CA 2006. [2] R. Malseed, F. J. Goldstein, N. Bulkon, Pharmacoplogy (drug therapy and nursing considerations), 4th ed. Vol. 4(39), Lippencott Company, Philadelphia, PA 1995. [3] K. Kargoshaa, J. Pharm. Biomed. Anal. 2001, 26(2), 273.
TRM in its capsule dosage form was analyzed successfully by the developed spectroscopic methods with good mean percentage found.
[4] I. D. Meras, A. E. Mansilla, F. S. Lopez, M. J. R. Gomez, J. Pharm. Biomed. Anal. 2002, 27(1–2), 81.
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