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International Journal of Basic and Applied Research
ISSN - 2249-3352
Vol. 02 Issue-2 (December 2012) (63-67)
Degradation Studies on Telmisartan and RP - HPLC
Method for The Determination of in Pure and
Pharmaceutical Formulation
Mohd.gousuddin , S.appala raju , Mashood ahmad shah , Sultanuddin
1
Faculty of pharmacy Lincoln College University Malaysia .
2
Department of Pharmaceutical Analysis H.K.E.Society's College of Pharmacy
Sedam Road, Gulbarga (K.S.) India.
Email : [email protected]
Key-words:
Abstract: A simple, selective, precise and stability indicating
RP High Performance Liquid Chromatographic (HPLC) method of analysis of Telmisartan in pure and pharmaceutical dosage form was developed and validated products. Separation was achieved on an XTerra® RP 8, 4.6 x150mm and the mobile phase (Buffer: acetonitrile: methanol) (45:25:30) KH2PO4 & Triethaylamine pH 3.0 with ortho phosphoric acid buffer flow rate of 1 ml/min and UV detection at 285 nm. Comprehensive stress testing of telmisartarn was according to the International Conference on Harmonization (ICH) guideline Q1A (R2). The drug was subjected to acid hydrolysis, base hydrolysis, to apply stress conditions. There were no other co eluting, interfering peaks from excipients, impurities. The method was validated in terms of linearity, precision, accuracy, specificity, robustness, and solution stability. The linearity of the proposed method was investigated in the range of 20‐100 μg/ml. The values of correlation coefficient INTRODUCTION:
vasoconstrictor and aldosteronesecreting effects of angiotensin II by selectively blocking the binding of angiotensin II to the AT1 receptor in many tissues, such as vascular smooth muscle and the adrenal gland. Telmisartan is indicated for the treatment of hypertension. Chemically known as 4'-[(1,4'-di methyl-2'-propyl [2,6'-bi- biphenyl]-2-carboxylic acid Its empirical formula is C33H30N4O2, its molecular weight is 514.63.The molecular structure of Telmisartan Gousuddin et.al
International Journal of Basic and Applied Research
Vol. 02 Issue-2 (December 2012) (63-67)
The objective of this work was to develop an analytical HPLC procedure, which would serve as stability indicating assay method for Telmisartan. A thorough h literature survey revealed that the Reported analytical procedures describing a stability indicating HPLC method for Telmisartan were more economical. The drug stability test guidelines Q1A (R2) [4] EXPERIMENTAL WORK AND
CONDITION
Harmonization (ICH) requires that analytical Buffer solution: 6 g of Potassium dihydrogen
test procedures for stability samples should be phosphate was accurately weighed a dissolved fully validated and the assays should be stability indicating. The objective of this work was to Triethaylamine then adjust pH 3 with OPA develop inexpensive, simple and rapid stability indicating RP-HPLC methods which would be Mobile Phase: Buffer: Acetonitrile: Methanol
validated according to ICH guidelines. The Preparation of Standard Solution:
intermediate precision of the described methods of Telmisartan Working standard into a 10 MATERIALS AND METHODS:
Diluent and sonicate to dissolve it completely Labdhi Private Limited and Product Name: same solvent. (Stock solution).A series of Fisher scientific pvt. Ltd. Acetonitrile: - HPLC grade, Spectrochem pvt. Ltd. Milli-Q water: - It was purified by Millipore Corporation's prepared followed by a suitable dilution of system mfg Barnsead. Triethylamine: - AR stock solution with the mobile phase.
grade, Spectrochem Pvt Ltd,Orthophosphoric acid:-AR grade, Fisher scientific pvt. Ltd. Preparation Sample preparation:
Potassium Dihydrogen Phosphate: - AR grade, Merck Specialities Pvt. Ltd. 1 N Hydrochloric calculate the average weight. Accurately weigh acid: - Merck, 1 N Sodium hydroxide: - Merck, and transfer the sample equivalent to 20 mg of Telmisartan into a 10 mL volumetric flask. Add INSTRUMENT USED:
about 7 mL of diluent and sonicate to dissolve it completely and make volume up to the mark with photodiode array detector and Empower with diluent. Mix well and filter through 0.45μm software. The column used was XTerra® RP 8, 4.6 x150mm, 3.5 μ. Thermal Stability studies were performed in a dry air oven (Thermo labs, Stress Degradation studies:
Acid degradation:
CHROMATOGRAPHIC CONDITIONS:
10mg of Telmisartan Working standard into a 100mL volumetric flask.To it 10mL of 0.1N Hcl was added and sonicated for 5minutes. Refluxed Mobile Phase: Buffer: Acetonitrile: Methanol under heat at 60 degrees in a heating metal for 2 hours the sample solution was neutralized using Gousuddin et.al
International Journal of Basic and Applied Research
Vol. 02 Issue-2 (December 2012) (63-67)
The objective of this work was to develop an Table2 Mean values of system
analytical HPLC procedure, which would serve suitability parameters
as stability indicating assay method for Parameters
Telmisartan
Telmisartan. A thorough h literature survey revealed that the Reported analytical procedures describing a stability indicating HPLC method for Telmisartan were more economical. The drug stability test guidelines Q1A (R2) [4] Harmonization (ICH) requires that analytical test procedures for stability samples should be Linearity
fully validated and the assays should be stability These results indicate that the response indicating. The objective of this work was to is linear over the range of 20, 40, 60, 80, and100 develop inexpensive, simple and rapid stability indicating RP-HPLC methods which would be Precision
validated according to ICH guidelines. The injecting the standard solution of30 μg mL‐1 intermediate precision of the described methods precision(repeatability) was evaluated by performing six consecutive injections of the MATERIALS AND METHODS:
30 μg mL‐1 standard solution, giving a low Labdhi Private Limited and Product Name: retention time of the drug. The Telmisartan Fisher scientific pvt. Ltd. Acetonitrile: - HPLC grade, Spectrochem pvt. Ltd. Milli-Q water: - It was purified by Millipore Corporation's system mfg Barnsead. Triethylamine: - AR grade, Spectrochem Pvt Ltd,Orthophosphoric Ruggedness and robustness of the method
acid:-AR grade, Fisher scientific pvt. Ltd. Potassium Dihydrogen Phosphate: - AR grade, Merck Specialities Pvt. Ltd. 1 N Hydrochloric acid: - Merck, 1 N Sodium hydroxide: - Merck, determined by analyzing same sample at normal operating conditions and also by changing some INSTRUMENT USED:
operating analytical conditions such as column make, mobile phase composition, flow rate and with photodiode array detector and Empower analyst. The deliberate a aforementioned software. The column used was XTerra® RP 8, changes in parameters alter the result of 4.6 x150mm, 3.5 μ. Thermal Stability studies Telmisartan 0.01% to method precision study, were performed in a dry air oven (Thermo labs, and ruggedness of the method shows assay CHROMATOGRAPHIC CONDITIONS:
Stress condition/ duration/
% Degradation
Mobile Phase: Buffer: Acetonitrile: Methanol Alkaline/ 5 N NaOH /100 °C/2hr/solution/ 5N Gousuddin et.al
International Journal of Basic and Applied Research
Vol. 02 Issue-2 (December 2012) (63-67)
Table: 3 represent the ruggedness and
Limit of detection (LOD) and Limit of
robustness of the method.
Quantitation (LOQ)
Parameters
Normal (orginal)
Changed condition
concentrations were found to be 2.88 and 9.62 XTerra RP-C8;4.6 x 150mm; 3.5 Luna RP-C8 150 x 4.6 mm; Accuracy
established by recovery studies. Results indicate that the individual recovery of Telmisartan ranges from 100.3% to 101.9% with mean recovery of 100.9% and % relative standard deviation of 0.37%. The recovery of satisfactory as % relative standard deviation is not more than ± 2.0% and mean recovery between 99.0 ‐ 102.0%. Table: 4. represent %Concentration
(at specification
% Recovery*
Fig. 1: The simple chromatogram of
standard Telmisartan.
Analysis of the marketed formulation
99.22% with a % RSD of 0.87%. It was noted that no degradation of Telmisartan had occurred in the marketed formulation that was analyzed by this method. The low RSD value indicated the suitability of this method for routine analysis of Telmisartan in pharmaceutical dosage form.
CONCLUSION
p r e c i s e , s p e c i f i c , a c c u r a t e a n d stability‐indicating. Statistical analysis proves that the method is suitable for the analysis of Telmisartan as bulk drug and in Pharmaceutical Fig. 2: The simple chromatogram of test
formulation without any interference from the Telmisartan
excipients. The study we can conclude that the Telmisartan undergo degradation to different extent under different, above mentioned, stress Gousuddin et.al
International Journal of Basic and Applied Research
Vol. 02 Issue-2 (December 2012) (63-67)
conditions. In this study, the products formed resolved from the bulk drug response.
REFERENCES:
Elbert W. Anal Chem. 1961, 33, 93-94 [11] SL Prabu; T Singh; A Joseph; C Dinesh I n t e r n a t i o n a l C o n f e r e n c e o n Michael E, Schartz IS, Krull. Analytical Gousuddin et.al

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