Imad Osman Abu Reid et al / International Journal of Advances in Pharmaceutical Analysis 2017; 07(03): 21-23.

21

International Journal of Advances in Pharmaceutical Analysis

ISSN: 2277-9353 (Online)
Journal DOI: https://doi.org/10.7439/ijapa Research Article

Spectrophotometric Method for the Simultaneous Determination of

Pseudoephedrine and Triprolidine in Bulk and Tablet Forms
Imad Osman Abu Reid* and Tasneem Awad Widaa

Pharmaceutical Chemistry Department, Faculty of Pharmacy, Al Ribat National University, Khartoum -Sudan

QR Code *Correspondence Info:

Imad Osman Abu Reid
Pharmaceutical Chemistry Department,
Faculty of Pharmacy,
Al Ribat National University, Khartoum –Sudan

*Article History:
Received: 14/05/2017
Revised: 09/06/2017
Accepted: 09/06/2017
DOI: https://doi.org/10.7439/ijapa.v7i3.4160
Abstract
A spectrophotometric method was developed for the simultaneous determination of pseudoephedrine HCl (PSE)
and triprolidine HCl (TRI) in bulk and dosage forms. The method involved the determination of pseudoephedrine in the
presence of triprolidine using two wavelengths (257 nm & 290 nm). Beer’s law was obeyed in the concentration (152-760
μg/ml) and (6.4-32 μg/ml) with good linearity (0.9996 and 0.9996) for pseudoephedrine and triprolidine respectively. The
accuracy and the precision of the developed method were very good (RSD ˂ 2%). The validity of the proposed method was
confirmed through the statistical comparison of the obtained data with those of the official USP method.
Keywords: Spectrophotometry, Simultaneous, Triprolidine, Pseudoephedrine.
1. Introduction The combination of TRI and PSE in tablets and
Pseudoephedrine (PSE) is a direct and indirect- syrup dosage form is official in the United State
acting sympathomimetic. It is a stereoisomer of ephedrine Pharmacopeia, normal phase HPLC method on silica
and has a similar action, but has been stated to have less column using mixture of alcohol and 0.4 % ammonium
pressor activity and fewer CNS effects. Pseudoephedrine acetate solution (17:3 v/v) as mobile phase , with ultraviolet
and its salts are given orally for the symptomatic relief of detection at 254 nm was employed for the determination of
nasal congestion [1]. the two analytes [2]. Literature review revealed that only
Triprolidine hydrochloride (TRI), an alkylamine few methods have been developed for the determination of
derivative, is a sedating antihistamine with antimuscarinic the two drugs combination, first derivative
and mild sedative effects. It is used for the symptomatic spectrophotometry and high performance liquid
relief of allergic conditions including urticaria and rhinitis, chromatography [3], partial least-squares multivariate
and in pruritic skin disorders [1]. It is often used in calibration [4], second order derivative spectrophotometry
combination with pseudoephedrine hydrochloride for [5], proportional isoabsorptive point spectrophotometric
rhinitis and in other compound preparations for the method [6], ratio spectra derivative spectrophotometry,
symptomatic treatment of coughs and the common cold [1]. derivative spectrophotometry and Vierordt’s method [7].
The chemical structures of triprolidine and The aim of the present work was to develop a
pseudoephedrine are shown in Figure 1. simple, sensitive and accurate spectrophotometric method
for the simultaneous determination of pseudoephedrine and
triprolidine in bulk and tablet dosage form.

2. Experimental
2.1 Materials and Instruments
Triprolidine (TRI) Pseudoephedrine (PSE) Pseudoephedrine HCl and triprolidine HCl
Fig 1: Chemical structures of triprolidine and
pseudoephedrine working standards (99.6% and 99.5%, respectively) were
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Imad Osman Abu Reid et al / Simultaneous Determination of Pseudoephedrine and Triprolidine in Bulk and Tablet Forms 22
kindly provided by Blue Nile Pharmaceuticals, Sudan. nm with corresponding specific absorptivity values 201.7
Trifed tablets (Al-Hikma Pharmaceutical Industry- Jordon): and 284.12, respectively. Triprolidine was found to
labeled to contain 60mg of pseudoephedrine hydrochloride interfere with pseudoephedrine absorbance only at the
and 2.5mg of Triprolidine hydrochlorides were purchased wavelength 257 nm; where pseudoephedrine has specific
from local market. absorptivity value of 8.10 (Fig. 2).
Hydrochloric acid analytical grade was purchased
from Scharlau Chemie, Spain.
Hydrochloric acid solution 0.1 M was used as a
diluent and solvent throughout the analysis.
UV spectrophotometric studies were carried out on
Shimadzu UV-1800 (Koyoto, Japan).
2.2 Samples and standard solutions preparation
2.2.1 Stock standard solutions
Stock standard solutions of TRI (160 μg/ml) and
PSH (3800 μg/mL) were prepared by accurately weighing
and dissolving about 8 mg TRI and 190 mg PSE into two
separate 50 ml volumetric flasks with 0.1N HCl.
2.2.2 Linearity standards
Figure 2: Absorption spectra of Triprolidine HCl (A) 30
Separate linearity standards of two analytes were
µg/ml and Pseudoephedrine HCl (B) 750 µg/ml
prepared by proper dilution of suitable aliquots from their
corresponding stock standard solutions with 0.1 HCl to give These findings were used to calculate the
concentration in the range of (6.4-32 μg/ml) and (152-760 concentration of the two analytes. Since at 290 nm the
μg/ml) for TRI and PSE, respectively. Absorbance values absorbance of triprolidine is free from interference by
were measured at 257 nm and 290 nm. The absorbance pseudoephedrine; its concentration was calculated from
values obtained at 257 nm and 290 nm were plotted against equation 1.
the corresponding TRI and PSE concentrations.
2.2.3 Sample preparation
CTRI = ATRI /A1%
1 cm 𝑙
A total of twenty tablets were accurately weighed,
Eq.1 (at 290 nm)
powdered and mixed well. A quantity of the resulted
powder equivalent to one tablet was weighed and
At the wavelength of 257 nm the sample
transferred into a 100 ml volumetric flask , the final
absorbance is the sum of the absorbance due to
volume was adjusted with 0.1 N HCl. The solutions were
pseudoephedrine plus the contribution from triprolidine;
sonicated for 15 min then filtered using 0.45 μ filter.
accordingly it is possible to calculate the concentration of
2.2.4 Laboratory synthetic mixtures
pseudoephedrine from the total absorbance at 257 nm using
Five laboratory synthetic mixtures containing
equation 2.
different amounts of TRI and PSE were prepared by proper
dilution of different aliquot volumes from their standards
Am = A1% 1%
1 cm PSE l CPSE+ A1 cm TRI l CTRI
stock solutions in 50 ml volumetric flasks using 0.1 N HCl.
and,
2.3 Procedure
APSE = Am – ATRI
2.3.1 Estimation of Wavelengths
Five ml of each stock standard solution were CPSE = (Am – (A1% 1%
1 cm TRI l CTRI)) /A1Ccm PSE

transferred to a separate 25 ml volumetric flasks. The Eq. 2 (at 257 nm)

volumes of the above solutions were completed to marks
using 0.1 M HCl. The resultant solutions were scanned Where: Am is the absorbance of the mixture; 𝐴1% 1 𝑐𝑚 is the

between 220-320 nm ranges. The wavelengths were specific absorptivity for TRI and PSE; l is the cell path
determined and their corresponding specific absorbance length (= 1 cm).
was calculated. 3.2 Linearity
Beer’s law was obeyed in the concentration range
(6.4-32 μg/ml) and (152-760 μg/ml) for TRI and PSE,
3. Results and discussion
3.1 Estimation of analytical wavelengths respectively. Table 1 reveals the statistical data for the
The UV spectrum of triprolidine showed regression equations of the proposed method.
absorbance at two wavelengths, namely 257 nm and 290
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Imad Osman Abu Reid et al / Simultaneous Determination of Pseudoephedrine and Triprolidine in Bulk and Tablet Forms 23
Table 1: Regression analysis data Table 4: Results of the proposed method compared to
PSE TRI the official method
Wavelength 257 nm 257 nm 290 nm % content t - calculated
Concentration range ± sd (t - tabulated)
(µg/ml) 152-760 6.4-32 Proposed Triprolidine 102.68
1.69 (2.57)
Slope (b) 0.00081 0.0201 0.0284 method (0.75)
Intercept (a) 0.0046 -0.0142 -0.0021 Pseudoephedrine 102.79
2.36 (2.57)
Correlation coefficient (r2) 0.9996 0.9997 0.9996 (0.70)
Standard deviation of the 0.0002 Official Triprolidine 102.00
slope (sb) 8.11x10-6 0.0002 method (0.69)
Standard deviation of the 0.0035 Pseudoephedrine 101.50
intercept (sa) 0.002 0.0029 (0.68)
3.3 Precision
The precision of the developed method was
4. Conclusion
evaluated by the results obtained from between-days The proposed method was proved to be simple,
(intermediate precision) and within-day data (repeatability) selective, precise and sensitive for the determination of
of six replicate determinations of samples containing 100% triprolidine and pseudoephedrine in bulk form and tablet
of their corresponding expected concentrations in the forms. Statistical and analytical validation of the results,
pharmaceutical product. The relative standard deviations using λ = 257 and 290 nm, confirmed that the simultaneous
(RSD) of their recoveries were determined. The observed determination could be used as an alternative method for
RSD levels (Table 2), which were below 2%, were the routine analysis of both drugs in quality control
considered satisfactory. For verification of precision the laboratories.
process was repeated on another day using fresh reagents References
and samples (intermediate precision). This evidenced that [1]. Sweetman S., Martindale: The Complete Drug
the outcome of the determination was statistically similar Reference 36th ed.UK: The Pharmaceutical Press. 2009
regardless the day of the assay and the reagents preparation. [2]. The United States Pharmacopoeia Convention. United
Table 2: Precision of the proposed method States Pharmacopoeia/ National Formulary INC. 24th
% of label claim ed. Rockville, MD; 2010.
Parameter Triprolidine Pseudoephedrine [3]. Madhuri A Hinge, K. R. Patel, Rajvi J. Mahida.
Day 1 Day 2 Day 1 Day 2 Spectrophotometric and High Performance Liquid
mean ( n =6) 102.68 103.00 102.79 102.94 Chromatographic Determination (HPLC) of
STDEV 0.75 0.72 0.70 0.93 Triprolidine and Pseudoephedrine Hydrochloride in
RSD% 0.73 0.76 0.68 1.02 Tablet Dosage Form. Pharm Methods, 2015; 6(2):87-
3.4 Recovery 93.
The proposed method was applied for the [4]. Onmez O, A , Bozdogan A , Kunt G, Div Y.
determination of the two analytes in five laboratory Spectrophotometric multicomponent analysis of a
synthetic mixtures containing different amounts of TRI and mixture of triprolidine hydrochloride and
pseudoephedrine hydrochloride in pharmaceutical
PSE. The mean content percent of five independent
formulations by partial least-squares multivariate
analyses for TRI and PSE were found to be 98.60 ± 0.65% calibration. Chem. Anal, 2007; 52(1):135-140.
and 101.28 ± 1.09%, respectively; n=5 (Table 3). [5]. Sriphong L, Chaidedgumjorn A, Chaisuroj K.
Table 3: Recovery data of the synthetic mixtures Derivative spectrophotometry applied to the
Triprolidine HCl Pseudoepherdine HCl determination of triprolidine hydrochloride and
% %
µg/ml µg/ml pseudoephedrine hydrochloride in tablets and
Content Content
Theoretical Actual Theoretical Actual dissolution testing. WASET, 2009; 32:569-573.
18.13 17.83 98.31 242.28 248.93 102.75
13.60 13.37 98.34 323.04 324.80 100.55 [6]. MoharanA R, kawathekar N, chaturvedi S.
13.60 13.36 98.21 242.28 247.49 102.15 simultaneous spectrophotometric estimation of
18.13 18.09 99.77 323.04 324.52 100.46 triprolidine hydrochloride and pseudoephedrine
22.67 22.30 98.37 403.80 405.87 100.51 hydrochloride in pharmaceutical dosage form. Indian
mean 98.60 mean 101.28 Journal of Pharmaceutical Sciences. 1996; 58(3):93-
RSD% 0.65 RSD% 1.09
95.
The validity of the method was further assessed by
[7]. Dinc E, Onur F. Comparison of the ratio spectra
comparing the statistical results obtained with those of the derivative spectrophotometry, derivative
official USP liquid chromatography method. As the spectrophotometry and Vierordt's method applied to
calculated t- values were less than tabulated ones (n =6, quantitative analysis of pseudoephedrine hydrochloride
P=0.05), the result of the developed method can be and triprolidine hydrochloride in tablets. STP Pharma
considered as accurate and precise as the official liquid Sciences. 1998; 8(3): 203-208.
chromatographic method (Table 4).
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