ACCENT JOURNAL OF ECONOMICS ECOLOGY & ENGINEERING
Peer Reviewed and Refereed Journal, ISSN No. 2456-1037, IMPACT FACTOR: 7.98, (INTERNATIONAL JOURNAL) Vol. 05, Issue 03, March 2020 Available Online: www.ajeee.co.in/index.php/AJEEE
120
DIFFERENTIAL PULSE POLAROGRAPHY WAS UTILIZED TO ESTIMATE THE AMOUNT OF TEGASAROD MALEATE
Revuri Dinesh Reddy
Asst. Professor, Department of Pharmacology, Princeton College of Pharmacy, Hyderabad, Telangana, India
Durgaiah Gandamalla
Asst. Professor, Department of Pharmacology, Princeton College of Pharmacy, Hyderabad, Telangana, India
Abstract - The hydrogen peroxide solution-treated tegaserod maleate can be estimated using a highly sensitive differential pulse polarographic method.
The oxidized product at the hanging mercury drop electrode could be quantitatively reduced using differential pulse polarography mode, making the oxidation of tegaserod maleate reversible. The measurement was restricted to 0.1ng/ml. In the presence of 0.1M potassium chloride as the supporting electrolyte, the voltametric peak was located at -1.05 volts.
Tegaserod maleate in its tablet form could be successfully analyzed using this method.
Keywords: Hanging mercury drop electrode, differential pulse polarography.
1 INTRODUCTION
Tegaserod maleate (TM), 3,5- methoxy-1H-indole-3-yl-
methylene)-N-pentylcarbazimida- mide hydrogen maleate, is a selective partial agonist of the 5- HT4 receptor that has a positive effect on the digestive system.
There is no official Pharmacopoeia for the drug. There are a few
HPLCMS, HPLC, and
spectrophotometric methods for analyzing TM in plasma and formulations, according to a comprehensive literature review.
Voltametry provides a collection of highly sensitive and selective techniques. These methods have been used to analyze pharmaceutically relevant compounds in a few reports that are currently available in the
literature. After being treated with hydrogen peroxide, the bulk and tablet formulations of TM were analyzed using differential pulse polarography in this study.
A Metrohm 757 Computrace VA voltameter connected to a PC was utilized for voltametric estimations. The multimode anode Metrohm stand was utilized in hanging mercury drop and dropping mercury drop cathode mode. A platinum wire auxillary electrode and a saturated calomel electrode served as the final two components of the three-electrode system. Following the IP procedure, the aqueous 0.1 M potassium chloride was prepared.
Water that had been twice distilled
ACCENT JOURNAL OF ECONOMICS ECOLOGY & ENGINEERING
Peer Reviewed and Refereed Journal, ISSN No. 2456-1037, IMPACT FACTOR: 7.98, (INTERNATIONAL JOURNAL) Vol. 05, Issue 03, March 2020 Available Online: www.ajeee.co.in/index.php/AJEEE
121 was used to make all of the aqueous solutions.
As a gift sample from the Torrent Research Centre in Ahmedabad, standard tegaserod maleate was utilized without any purification. The local pharmacy supplied the commercial tablet formulation Tegib-6 from Torrent Pharmaceuticals in Ahmedabad, India.
Ten milligrams of standard TM were refluxed for 30 minutes at 80° with 5 ml of 3% H2O2. After being brought to room temperature, the flask was boiled once more for 15 minutes without the reflux condenser to remove the excess H2O2. After cooling, 10 milliliters of methanol were added to the solution. To get rid of any remaining hydrogen peroxide, the solution was boiled for three to four minutes more. The solution was cooled once more and diluted with methanol to 100 milliliters. A stock solution of 1 g/ml was produced by further diluting the solution. Similar preparations were used for other concentrations' standard solutions.
The differential pulse mode was utilized with a pulse amplitude of 50 mV and a drop time of 0.8 s. Twenty milliliters of 0.1 M KCl were taken in the polarographic cell, and nitrogen was purged through the solution for 300 s. An aliquot of 1 l–1 ml from the standard TM solution was then added to the KCl, and
nitrogen purging was continued for 10 s. After a 10 s sweep equilibration, the polarogram was recorded. Twenty tablets (Tegib-6 from Torrent Pharmaceuticals) were ground into a fine powder and weighed. 10 mg of powder was weighed, and 5 milliliters of 3%
H2O2 were used to treat it as previously mentioned. The standard addition method was used to estimate by adding the standard TM solution at two levels.
We attempted to develop a voltametric method using a glassy carbon electrode after discovering that TM is susceptible to oxidation.
However, our attempts to obtain a voltammogram using either the anodic range of DME or the glassy carbon electrode were unsuccessful. However, a sharp polarogram in the cathodic range of a dropping mercury electrode was observed in the TM solution that had already been treated with hydrogen peroxide. As a result, a hanging mercury drop electrode (HMDE) was used to develop the polarographic method in the differential pulse polarographic mode. At -1.05 V, the peak was observed (fig. 1). Various media, including Britton-Robinson buffers (pH 6-12), phosphate buffer (pH range 2-7), and 0.1 M lithium chloride, were tested to see how the composition of the supporting electrolyte affected the shape of the TM polarogram. However, 0.1 M KCl produced the best results, with a polarogram that was sharp
ACCENT JOURNAL OF ECONOMICS ECOLOGY & ENGINEERING
Peer Reviewed and Refereed Journal, ISSN No. 2456-1037, IMPACT FACTOR: 7.98, (INTERNATIONAL JOURNAL) Vol. 05, Issue 03, March 2020 Available Online: www.ajeee.co.in/index.php/AJEEE
122 and clearly defined. The effect of deposition potential on pulse amplitude, voltage step time, and working parameters of differential pulse polarography were investigated with 0.1M KCl as the supporting electrolyte. With a deposition potential of -0.5 V, a deposition time of 68 s, a drop size
of 4, an equilibration time of 10 s, a voltage step of 0.006 V, a pulse amplitude of 0.05 s, and a voltage step time of 0.4 s, the optimal parameters are shown in Table 1.
Triton-X 100 or any other surfactant was not evaluated because the polarogram was smooth.
Fig. 1 Differential pulse polarogram of tegaserod maleate The three polarograms are for three different concentrations (0.2, 0.4 and 0.6
μg/ml) of tegaserod maleate solution.
Table 1 Working conditions for differential pulse polarographic analysis of tegaserod maleate
Six determinations were evaluated for their reproducibility of polarographic response, and the relative standard deviation was found to be 0.56%. The estimated limit of quantification was 0.1 g/l, or 0.1 ng/ml. The standard addition method was used to
estimate TM in pharmaceutical preparations using this method (fig. 2). The outcomes showed 100.32±0.68% recuperation recommending results to be in great concurrence with the name guarantee. Although it is an indirect method, the method is
ACCENT JOURNAL OF ECONOMICS ECOLOGY & ENGINEERING
Peer Reviewed and Refereed Journal, ISSN No. 2456-1037, IMPACT FACTOR: 7.98, (INTERNATIONAL JOURNAL) Vol. 05, Issue 03, March 2020 Available Online: www.ajeee.co.in/index.php/AJEEE
123 extremely sensitive and can be used to monitor extremely low TM
concentrations.
Fig. 2: Analysis of tegaserod maleate by standard addition method The standard addition was done at two levels.
REFERENCES
1. Budavari S. editors. In; The Merck Index, 13th ed. Whitehouse Station NJ: Merck and Co.; 2001.
p. 1496.
2. Indian Pharmacopoeia, 4th ed.
New Delhi: The Controller of Publications; 1996.
3. British Pharmacopoeia, London:
Her Majesty’s Stationary Office;
2002.
4. United States Pharmacopoeia, 28th ed. Rockville, MD: The United States Pharmacopoeial Convention Inc.; 2001.
5. Zhou H, Khaliliesh S, Campestrine J, Appel-dingemanse S, Lachman L, Mcleod J. Effect of gastric pH on plasma concentration of tegaserod.
J Gastroenterol 2000;118:1206- 10.
6. Singh SS, Patel HV, Sharma K.
Estimation of tegaserod in human plasma by HPLC-Tandem mass spectroscopy and its application to bioequivalence study. Anal Chim Acta 2006;557:229-35.
7. Yang B, Gao MJ, Duan GL. Ion Pair RPLC of tegaserod maleate and its impurities in pharmaceutical formulation and in
dissolution studies.
Chromatographia 2006;63:431-6.
8. Rajput SJ, Raj HA. Assay of tegaserod maleate by difference spectroscopy. Indian J Pharm Sci 2007;69:114-5.
9. Rajput SJ, Raj HA.
Spectrophotometric estimation of tegaserod maleate in bulk drug and in tablet formulation. Indian J Pharm Sci 2007;69:314-6.
10. Inam R, Mercan H, Yilmaz E, Uslu B. Differential pulse polarographic determination of moxifloxacin hydrochloride in pharmaceutical and biological fluids. Anal Lett 2007;40:529-46.
11. Debnath C, Haslinger E, Likussar W, Micheliletsch A. Determination of the antimalarial drug artemether in the pharmaceutical preparations by differential pulse polarography. J Pharm Biomed Anal 2006;41:638-43.