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New Spectrophotometric Assay of Pyrantel Pamoate in Pharmaceuticals and Spiked Human Urine Using Three Complexing Agents

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85 views

New Spectrophotometric Assay of Pyrantel Pamoate in Pharmaceuticals and Spiked Human Urine Using Three Complexing Agents

keratitis

Uploaded by

Nurul Fatimah
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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DOI 10.

1007/s10812-015-0138-4
Journal of Applied Spectroscopy, Vol. 82, No. 3, July, 2015 (Russian Original Vol. 82, No. 3, May–June, 2015)

NEW SPECTROPHOTOMETRIC ASSAY OF PYRANTEL PAMOATE


IN PHARMACEUTICALS AND SPIKED HUMAN URINE USING
THREE COMPLEXING AGENTS

N. Swamy, K. N. Prashanth, and K. Basavaiah* UDC 535.243:615.45

Three simple, rapid, inexpensive, and highly sensitive spectrophotometric methods are described for the quantification
of pyrantel pamoate (PYP) in pure drug and formulations. The methods are based on the molecular charge-transfer
(CT) complexation reaction involving pyrantel base (PYL) as n-donor and iodine as σ-acceptor (I2, method A), and
2,4-dinitrophenol (DNP, method B) or picric acid (PA, method C) as π-acceptors. Spectrophotometrically, the CT
complexes showed absorption maxima at 380, 420, and 430 nm, for methods A, B, and C, respectively. Under optimum
conditions, Beer's law was obeyed over the concentration ranges 0.12–2.9, 0.12–3.75, and 0.12–2.9 μg/ml for methods
A, B, and C, respectively. The apparent molar absorptivity of the CT complexes at the respective λmax are calculated
to be 2.63 × 105, 6.91 × 104, and 1.73 × 105 l/mol·cm respectively and the corresponding Sandell sensitivity values
are 0.0009, 0.003, and 0.0012. The limits of detection (LOD) and quantification (LOQ) are calculated to be (0.02 and
0.07), (0.05 and 0.15), and (0.02 and 0.07) μg/ml with methods A, B, and C, respectively. The intra-day and inter-day
accuracy expressed as %RE and precision expressed as %RSD are less than 3%. The methods have been applied
to the determination of PYP in tablets, suspensions, and spiked human urine. Parallel assay by a reference method
and statistical analysis of the results obtained show no significant difference between the proposed methods and the
reference method with respect to accuracy and precision, as evident from the Student’s t and variation ratio tests. The
accuracy of the methods has been further ascertained by recovery tests via the standard addition technique.

Keywords: pyrantel pamoate, assay, spectrophotometry, pharmaceuticals, charge-transfer complexation.


Introduction. Pyrantel pamoate (PYP), chemically known as [1,4,5,6-tetrahydro-1-methyl-2-[2-(2-thienyl) ethenyl]
pyrimidine]:

could be effectively used to control serum mineral levels in children with intestinal parasitic infection [1]. Pyrantel pamoate
shows maximum activity towards pigs as compared with its citrate form, i.e., pyrantel citrate [2].
Another interesting aspect of PYP is the improvement in appetite and growth in helminth-infected children 3 and
7 weeks after a single dose of PYP [3], and it is very effective against A. lumbricoides, hookworms, T. orientalis, and
E. Vermicularis [4, 5]. Pyrantel pamoate is the subject of a monograph in the United States Pharmacopoeia (USP) [6], which
describes chromatographic methods for both bulk drug and its formulations.
An extensive literature survey reveals that several techniques have been reported for the assay of PYP in pharmaceutical
formulations, which include high-performance liquid chromatography (HPLC) [7–15], high-performance thin layer
chromatography (HPTLC) [16, 17], UV-spectrophotometry [18–21], spectrofluorimetry [22], voltammetry [23–25], and
_____________________
*
To whom correspondence should be addressed.

Department of Chemistry, Manasagangothri, University of Mysore, Mysore-570 006, Karnataka, India; e-mail:
[email protected]. Abstract of article is published in Zhurnal Prikladnoi Spektroskopii, Vol. 82, No. 3, p. 479,
May–June, 2015.

502 0021-9037/15/8203-0502 ©2015 Springer Science+Business Media New York


ion-selective electrode-potentiometry [26]. However, many of these methods suffer from limitations such as the need for
sophisticated and expensive instruments and skilled manpower, which are not always found in many laboratories of developing
and underdeveloped countries. In contrast, visible spectrophotometric methods offer high sensitivity, low detection limit,
easy operation, and use of simple instrumentation.
Few visible spectrophotometric methods based on condensation, redox, and complexation reactions are found in
the literature. PYP was assayed based on its reaction with malonic acid and acetic anhydride at elevated temperature [22].
Based on the reduction of FC reagent by PYP in alkaline medium to a blue colored product, a method was developed
by Basavaiah and Prameela [27]. Four methods were described by Lakshmi and Reddy [28] based on the formation of
colored charge-transfer complex between drug and chloranil, or by the reduction of FC reagent or by reacting with the
oxidant N-bromosuccinimide (NBS) or KMnO4 and using the dye celestein blue or cresyl fast violet acetate. The drug in the
concentration range 25–400 μg/ml was as assayed based on its reaction with chloranil in dioxane medium where the resulting
CT complex [29] was measured at 560 nm. Extractive spectrophotometric methods have also been reported for the estimation
of drug in dosage forms [30] based on colored ion-pair complex of the drug with dyes like wool fast blue, supracen violet 3B
and azocarmine G.
However, many of these methods suffer from one or other disadvantages. Methods based on reduction and CT
complex formation [27–29] are less sensitive with a narrow linear range of applicability. Many other methods are time
consuming and cumbersome since they involve the use of multi-agent and multi-step reactions [28] or require elevated
temperature [22], and hence prone to inaccuracy and imprecision. The extractive spectrophotometric methods [30], though
sensitive, suffer from such disadvantages as tedious and time-consuming extraction step, critical dependence on pH, and
aqueous-organic phase ratio. They are also prone to inaccuracy owing to incomplete extraction of the ion-pair or formation
of emulsion between the solvent and the drug solution.
There is, therefore, a need for simple, rapid and sensitive methods for systematic control procedures aimed at ensuring
the quality of dosage forms, which are made available for public use. This study was therefore undertaken to develop methods
that would overcome most of the above shortcomings. The methods are based on the formation of CT complex of the drug
with acceptors such as iodine, dinitrophenol, and picric acid. The results obtained are promising and demonstrate the utility
of the methods in determining the content of active substance in pharmaceutical formulations.
Experimental. A Systronics model 166 digital spectrophotometer (Systronics, Ahmedabad, Gujarat, India) equipped
with 1-cm matched quartz cells was used for all absorbance measurements.
Pharmaceutical grade PYP (99% purity) was received as a gift from IPCA pharmaceutical company, Ratlam, India,
and was used as received. Nemocid tablets and Nemocid oral suspension (IPCA laboratories Ltd., Ratlam, India) were
purchased from local commercial sources. A human urine sample was collected from a healthy male aged about 29 years.
All chemicals used were of analytical reagent grade, and HPLC grade organic solvents were used throughout the
investigation. Solutions of 0.5% iodine (I2, Merck, Mumbai, India), 0.1% 2,4-dinitrophenol (DNP, Merck, Mumbai, India),
or 0.05% picric acid (S.D. Fine-Chem, Mumbai, India) were prepared separately in chloroform for methods A, B, or C.
A stock standard solution containing 100 μg/ml PYL (base) was prepared by dissolving 28.57 mg of pure drug in
10 ml N,N-dimethylformamide (DMF) in a 125 ml separatory funnel. Then 5 ml of 1 M NaOH was added, followed by 60 ml
(20 × 3) chloroform, and the content was shaken for 15 min. The lower organic layer was collected in a beaker containing
about 2 g of anhydrous sodium sulphate. The anhydrous organic layer was transferred into a 100 ml calibrated flask and
diluted to the volume with chloroform to get 100 μg/ml with respect to PYL (pamoate-free pyrantel). This was diluted
appropriately with the same solvent to get a working concentration of 2 μg/ml PYL and used in all methods.
Assay Procedures. Method A (Using I2). Different aliquots of 0.1, 0.25, 0.5, 1.0, 1.5, 2.0, and 2.5 ml of standard
PYL solution (2 μg/ml) were accurately transferred into 5 ml standard flasks using a microburette, and the total volume was
adjusted to 2.5 ml by adding an adequate quantity of chloroform. One ml of 0.5% iodine was added to each flask and the
mixture was diluted to the volume with chloroform and mixed well. The absorbance of each solution was measured at 380 nm
against a reagent blank after 5 min.
Method B (Using DNP). Aliquots of 0.1, 0.25, 0.5, 1.0, 1.5, 2.0, 2.5, 3.0, and 3.25 ml of standard PYL solution
(2 μg/ml) were accurately added to 5 ml calibrated flasks using a microburette, and the total volume was adjusted to 3.25 ml
with chloroform. With 1 ml of 0.1% DNP added to each flask, the mixture was diluted to the volume with chloroform and mixed
well. After 5 min the absorbance of each solution was measured at 420 nm against a reagent blank prepared simultaneously.
Method C (Using PA). Into a series of 5 ml volumetric flasks, 0.1, 0.25, 0.5, 1.0, 1.5, 2.0, and 2.5 ml of the standard
PYL solution (2 μg/ml) were accurately added using a microburette, and the total volume was adjusted to 2.5 ml with

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