ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF SIMULTANEOUS ESTIMATIO

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apmc college of pharmaceutical education and research, himatnagar,9824640052.

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Analytical Method Development and Validation of Simultaneous Estimation of Amlodipine besylate and Indapamide in Combined Dosage Form.:

Analytical Method Development and Validation of Simultaneous Estimation of Amlodipine besylate and Indapamide in Combined Dosage Form. Prepared By: Shah Ghanshyam R . M.Pharm SEM-III Enrollment No.03 Guided By: Dr. Dushyant Shah Pricipal of APMCCPER DEPARTMENT OF QUALITY ASSURANCE APMCCPER, HIMMATNAGAR Introduction to dissertation

Contents:

Contents Introduction Drug profile Literature review Aim of Work Plan of work References

Introduction :

Introduction Hypertension Hypertension is the most common cardiovascular disease. The prevalence of hypertension increases with advancing age; for example, about 50% of people between the ages of 60 and 69 years old have hypertension, and the prevalence is further increased beyond age 70 . Hypertension is defined conventionally as a sustained increase in blood pressure ≥ 140/90 mm Hg, a criterion that characterizes a group of patients whose risk of hypertension-related cardiovascular disease is high enough to merit medical attention. Actually, the risk of both fatal and nonfatal cardiovascular disease in adults is lowest with systolic blood pressures of less than 120 mm Hg and diastolic BP less than 80 mm Hg; these risks increase progressively with higher systolic and diastolic blood pressures.

Introduction (conti…):

Introduction ( conti …) Criteria for Hypertension in Adults BLOOD PRESSURE (MM HG) CLASSIFICATION Systolic Diastolic Normal <120 and <80 Pre-hypertension 120–139 or 80–89 Hypertension, stage 1 140–159 or 90–99 Hypertension, stage 2 ≥ 160 or ≥ 100

The various validation parameters of Analytical methods::

The various validation parameters of Analytical methods: Accuracy Precision (repeatability and reproducibility) Linearity and range Limit of detection (LOD)/ limit of quantification (LOQ) Selectivity/ specificity Robustness/ ruggedness Stability and system suitability studies. Introduction ( conti …)

Drug profile:

Drug profile SR NO PARAMETER AMLODIPINE BESYLATE INDAPAMIDE 1. STRUCTURE 2. FLOUROSCENCE Excitation : 375 nm Emission: 480 nm Excitation : 284 nm Emission: 356 nm 3. CHEMICAL NAME 2-[(2-Aminoethoxy)methyl]-4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine benzenesulfonate Benzamide , 3-( aminosulfonyl )-4-chloro- N -(2,3-dihydro-2-methyl-1 H -indol-1-yl)-. 4-Chloro- N -(2-methyl-1-indolinyl)-3-sulfamoylbenzamide [ 26807-65-8 ].

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SR NO PARAMETER AMLODIPINE BESYLATE INDAPAMIDE 3. CATEGORY Antihypertensive (Calcium channel blocker). Oral Antihypertensive (Diuretic). 4. SOLUBILITY Soluble in methanol, sparingly soluble in ethanol, slightly soluble in water. Soluble in methanol, ethanol, acetic acid, ethyl acetate, slightly soluble in ether, practically insoluble soluble in water. 5. MOLECULAR FORMULA C 20 H 25 ClN 2 O 5 . C 6 H 6 O 3 S C 16 H 16 ClN 3 O 3 S 6. MELTING POINT 195-204 0 C 160-162 0 C 7. MOLECULAR WEIGHT 567.05 g/mole 365.84 g/mole

Literature Review:

Literature Review AMLODIPINE BESYLATE : Official in Indian Pharmacopoeia 2010, assayed by liquid chromatography. Mobile phase - The upper layer of a mixture of 25 volumes of glacial acetic acid, 25 volumes of water and 50 volumes of methyl isobutyl ketone . INDAPAMIDE : Official in United State Pharmacopoeia, assayed by liquid chromatography. Mobile phase: water, acetonitrile, methanol and glacial acetic acid (650:175:175:1).

Literature Review (conti..):

Literature Review ( conti ..) AMLODIPINE BESYLATE Reported work Matrix Description Estimation of Amlodipine Besylate . Tablets Method- spectroflourimetry Condensation with Ninhydrine and phenylacetaldehyde in pH 7. Excitation wavelength 375 nm and emission maxima 480 nm. Estimation of Amlodipine Besylate. Tablets Method- spectroflourimetry Reaction with 7-chloro-4-nitro-2,1,3-benzoxadiazole (NBD- Cl ) in a buffered medium (pH 8.6) resulting in formation of a highly fluorescent product, which was measured fluorometrically at 535 nm (lambda(ex), 480 nm). Non official method:

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Reported work Matrix Description Simultaneous estimation of amlodipine and valsartan Tablet Method - spectro fluorimetry Native fluorescence at 455 nm (λ (Ex) 360 nm) and 378 nm (λ (Ex) 245 nm) for Amlodipine and Valsartan, respectively. Simultaneous estimation of amlodipine and nebivolol Tablet Method – HPLC Detector- UV Simultaneous estimation of Amlodipine and Nebivolol Hydrochloride Tablet Method – HPTLC Mobile phase - Methylene Chloride : Methanol : Ammonia ( 8.5:1:0.5 v/v ) Stationary phase - precoated plate of silica gel 60 F 254. Detection – at 285 nm. Simultaneous estimation of Amlodipine and Atorvastatin API Method – UV spectroscopy 1. Simultaneous equation using 361 nm and 246 nm as two analytical wavelengths for both drugs. 2. Q value analysis based on measurement of absorptivity at 238.8 nm (as an iso -absorptive point) and 246 nm.

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Reported work Matrix Description Simultaneous estimation of Losartan Potassium and Amlodipine Besylate Tablet Method – UV spectroscopy 1. Simultaneous equation using 208 nm and 237.5 nm as two analytical wavelengths for both drugs. Solvent – methanol. 2. Q value analysis based on measurement of absorptivity at 242.5 nm (as an iso -absorptive point) and 237.5 nm. Simultaneous estimation of Amlodipine Besylate and Olmesartan Medoxomil Tablets Method – RP HPLC Mobile phase - Acetonitrile and water in the ratio 60:40. Retention time – 6 min. Flow rate – 1 ml -1 . Detection – at 246 nm. Simultaneous estimation of Nebivolol hydrochloride and Amlodipine besylate API Method – UV spectroscopy 1. Simultaneous equation using 238 nm and 281 nm as two analytical wavelengths for both drugs. Solvent – methanol. 2. Simultaneous equation using 238 nm and 360 nm as two analytical wavelengths for both drugs.

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Reported work Matrix Description Simultaneous estimation of Nebivolol and Amlodipine besylate Tablet Method – UV-Absorption correction Method Wavelengths for Amlodipine are - 262 and 332.5 nm which are giving same absorbance. Wavelength for Nebivolol is – 262 nm. Simultaneous estimation of Nebivolol hydrochloride and Amlodipine besylate Tablet Method – UV-Q analysis method or Absorption ration method. Iso-absorptive point 268nm (λ1) λmax of one of the sample components 282nm (λ2) Simultaneous determination of Amlodipine besylate and Nebivolol hydrochloride Tablet Method – UV-Absorption correction method Determination of Amlodipine besylate at 365 nm using its absorptivity value and Nebivolol hydrochloride at 280 nm after deduction of absorbance due to Amlodipine besylate. Simultaneous estimation of Nebivolol and s-Amlodipine Tablet Method – UV- simple first derivative spectrophotometric method. Wavelength for S- Amlodipine is – 242 nm. Wavelength for Nebivolol is – 290 nm.

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Reported work Matrix Description Determination of atorvastatin and amlodipine simultaneously Tablet Method – rapid HPLC method Mobile phase - a mixture of acetonitrile and 0.03M phosphate buffer pH 2.9 (55:45% v/v). Detection - atorvastatin and amlodipine was carried out on dual g absorbance detector at 240 nm and 362 nm, respectively. Simultaneous estimation of Telmisartan and Amlodipine Tablet Method – UV- multi component mode of analysis Wavelengths assayed for both drugs are – 296 and 363 nm. Simultaneous estimation of amlodipine besylate and telmisartan Tablet Method – UV- multi wavelength analysis Wavelengths assayed for both drugs are – 298 and 360 nm.

Literature Review (conti..):

Literature Review ( conti ..) INDAPAMIDE Reported work Matrix Description Spectroflourimetry Assay API Method- spectroflourimetry With NaOH at 100 0 c, excitation at 284 nm and emission at 356 nm. Simultaneous estimation of Indapamide and Nebivolol hydrochloride Tablet Method- UV spectroscopy Simultaneous equations method at 241.6 nm (λ-max of Indapamide ) and 281.5 nm (λ-max of Nebivolol hydrochloride). Q-analysis method (Q-absorbance ratio) at 274 nm ( Iso -absorptive point) and 281.5 nm (λ-max of Nebivolol hydrochloride). Non-official methods:

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Simultaneous estimation of Perindopril and Indapamide Tablet Method – UV- Absorption correction method. λmax of Perindopril – 210.4 nm. λmax of Indapamide – 285.8 nm. Solvent – methanol. Simultaneous determination of Perindopril erbumine and Indapamide Method - H igh performance thin layer chromatographic (HPTLC) method. Mobile phase - Dichloromethane: Methanol: Glacial acetic acid in the ratio of 9.5:0.5:0.1 v/v/v. Stationary phase - plates precoated with silica gel 60 F 254 . Detection – at 215 nm. Quantitative estimation of Aceclofenac and Indapamide Tablet Method – UV-Colorimetric method. Reagent - Folin-Ciocalteu reagent. Aceclofenac forms a blue colored chromogen with the reagent, which shows absorbance maxima at 642.6 nm. Indapamide forms a green colored chromogen with the reagent, which shows absorbance maxima at 783.2 nm.

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Reported work Matrix Description A stability-indicating assay method for simultaneous determination of Telmisartan and Indapamide (forced degradation). Product - degraded Method – HPLC Column - Amazone C18, 5 microm , 150 x 4.6 mm Mobile phase - (Buffer: acetonitrile : methanol)= (45:25:30) KH 2 PO 4 & Triethaylamine pH 3.0 with ortho phosphoric acid buffer. Flow rate - 1.0ml/min Simultaneous estimation of Telmisartan and Indapamide API Method – RP HPLC. Mobile phase - Acetonitrile : 0.1M Potassium dihydrogen phosphatebuffer [60:40v/v]. Column - Hypersil Gold column [250×4.6mm; 5μm]. Flow rate – 1 ml/ min. Detection – at 237 nm.

Aim of Work:

Aim of Work To develop and validate, accurate and precise method for simultaneous estimation of AMLODIPINE BESYLATE and INDAPAMIDE using following technique. UV-Visible spectrophotometric method HPTLC Spectrofluotimetric Method To apply above methods for simultaneous estimation AMLODIPINE BESYLATE and INDAPAMIDE in combined marketed dosage form

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18 Plan of work

References:

References Indian Pharmacopoeia, 2007, Volume-II, the Indian Pharmacopoeia Commission, Ghaziabad, Govt. of India, Ministry of Health and Family Welfare, pp 741. United state pharmacopoeia, 30- National formulary 25. Chatwal A., Instrumental Method of Chemical Analysis, 15th edition, pp 215-219 ICH Q2A, Text on Validation of Analytical Procedure, 1995 ICH Q2B, Validation of Analytical Procedure Methodology, 1997. Joel GH, Lee EL (ed.), Goodman and Gilman’s, The Pharmacological Basis of Therapeutics, 10 th edition, International edition, New York: The MC Graw Hill companies Inc.; 2001. Abdel- Wadood HM , Mohmed NA, Mahmoud AM, “Validated Spectrofluorometric methods for determination of amlodipine besylate in tablets” Spectrochimica Acta Part A molecular and bimolecular spectroscopy . 2008 70(3), 564-70. Epub 2007 Aug 11.

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Shaalan R A, Belal T S, “Simultaneous Spectrofluorimetric determination of amlodipine besylate and valsartan in their combined tablets” Drugs Test Anal . 2010 2(10), 489-93. Sharma D, Jain A, Shrivastav A, “Simultaneous estimation of Amlodipine besylate and Nebivolol hydrochloride in tablet forms by RP-HPLC using ultraviolet detection” Pharmamethods . Jan-March 2011 , 2. Dhandapani B, Anjaneyulu1 N, Venkateshwarlu Y and Rasheed SH, “ HPTLC Method Development and Validation for the Simultaneous Estimation of Amlodipine Besylate and Nebivolol Hydrochloride in tablet dosage form” Journal of Pharmacy Research . 2010, 3. Patel SR, Patel SM, Patel JI, Patel PU, “Development and Validation of High-Performance Thin-Layer Chromatography Method for Determination of Nebivolol and Amlodipine in Combined Dosage Forms” Journal of Pharmacy Research. 2010 , 3(9), 2273-2275. Patil PR, Rakesh SU, Dhabale PN, and Burade KB, “Simultaneous UV Spectrophotometric Method for Estimation of Losartan Potssium and Amlodipine Besylate in Tablet Dosage Form.” Asian J. Research Chem . 2009 2(1).

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Ramesh D, Ramakrishna S, “New spectrophotometric methods for simultaneous determination of Amlodipine besylate and Atorvastatin calcium in tablet dosage forms” International Journal of Pharmacy and Pharmaceutical sciences. 2010 2, Issue 4. Patil PS, More HN, Pishwikar SA, “RP-HPLC method for simultaneous estimation of Amlodipine besylate and Olmesartan medoxomil from tablet” International Journal of Pharmacy and Pharmaceutical Sciences . 2011 3. Mishra P, Shah K, Gupta A, “ Spectrophotometric methods for simultaneous estimation of Nebivolol hydrochloride and Amlodipine besylate in tablets” International Journal of Pharmacy and Pharmaceutical Sciences Oct-Dec. 2009 1 Issue 2. Patel SA, Patel PU, Patel NJ, “Absorbance correction method for simultaneous determination of Nebivolol and Amlodipine besylate in combined tablet dosage form” International Research Journal of Pharmacy 2011 2 (8), 92-95. Giri CK, Kondawar MS and Chougule DD, “Simultaneous estimation of Nebivolol hydrochloride and Amlodipine besylate in combined tablet dosage form by Q-analysis method” International Research Journal of Pharma . Research and Development 2010 2.

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Chandnani VC, Gupta KR, Chopde CT, Kunjwani HK, Manikrao AM and Shivhare SC, “Simultaneous UV- spectrophotometric determination of Amlodipine besylate and Nebivolol hydrochloride in tablet dosage form” International Journal of ChemTech Research Jan-Mar 2010 2, 69-73. Joshi HV, Patel JK, Patel MP and Wankhede S, “Simultaneous estimation of Nebivolol and S- Amlodipine in tablets by UV- Spectrophotometry ” DER Pharma Chemica online Journal of Medicinal Chemistry, Pharmaceutical Chemistry and Computational Chemistry . Rajeswari KR, Sankar GG, Rao AL and Seshagirirao JVLN, “RP-HPLC method for the simultaneous determination of Atorvastatin and Amlodipine in tablet dosage form” Indian Journal of Pharmaceutical Sciences 2006 68, Issue-2, 275-277. Patel PU and Patel HP, “Two Spectroscopic Methods for the Simultaneous Estimation of Indapamide and Nebivolol Hydrochloride in Combined Dosage Form”, International Journal of Pharmaceutical Research 2011 3, Issue 2, 55-57. Joseph J, Philip B and DR. M. Sundarapandian M, “Method development and validation for simultaneous estimation of Perindopril Erbumine and Indapamide by RP-HPLC in pharmaceutical dosage forms” International Journal of Pharmacy and Pharmaceutical Sciences 2011 3.

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Modi DK and Patel CN, “Development and Validation of Spectrophotometric Method for Simultaneous Estimation of Perindopril and Indapamide in Combined Dosage form by Absorbance Correction Method” International Journal of PharmTech Research Jan-Mar 2010 2, 411-416. Dewani MG, Bothara KG, Madgulkar AR and Damle MC, “Simultaneous estimation of Perindopril Erbumine and Indapamide in bulk drug and tablet dosage form by HPTLC” International Journal of Comprehensive Pharmacy Pharmacie globale 2011 , 1 (01). Singhvi I and Goyal A, “Visible spectrophotometric estimation of Aceclofenac and Indapamide from tablets using folin-ciocalteu reagent” Indian Journal of Pharmaceutical Sciences 2007 69, Issue-1, 164-165. Patel AR and Chandrul KK, Method development, “Validation and stability study for simultaneous estimation of telmisartan and indapamide by reverse phase-high performance liquid chromatography in pure and marketed formulation” International Journal on Pharmaceutical and Biomedical Research (IJPBR) 2011 2(1), 4-16. Munot NM, Ghante MR, Deshpande AS, and Gaikwad PV, “Development and Validation of RP-HPLC Method for Simultaneous Estimation of Indapamide and Telmisartan ” Journal of Pharmacy Research 2010 , 3(12), 2941-2943.

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Suresh kumar GV, Rajendraprasad Y, “Development and validation of reversedphase HPLC method for simultaneous estimation of Telmisartan and Amlodipine in tablet dosage form” International Journal of Pharmacy and Pharmaceutical Sciences 2010 2, Issue 3. Kondawar MS, Kamble KG, Raut KS andMaharshi KH, “UV Spectrophotometric estimation of Amlodipine besylate and Telmisartan in Bulk drug and Dosage form by Multiwavelength Analysis” International Journal of ChemTech Research July-Sept 2011 3, 1274-1278. Muthu AK, Sankala R, Chidalla.SD and Manavalan R, “Simultaneous estimation of Telmisartan and Amlodipine by uv Spectrophotometric method using multi component Mode of Analysis” International Research Journal of Pharmacy , 2011 2, 175-180. Grebow PE, Johnston MM and Mellett LB, “ Indapamide : Measurement by a Flourescence assay” Current Medical Research and Opinion 1977 5, 9-12. October 2011, http://chemicalland21.com/lifescience/uh/INDAPAMIDE.htm November 2011, http://www.drugbank.ca/drugs/DB00808 November 2011, http://www.drugbank.ca/drugs/DB00381 October2011, http://chemicalland21.com/lifescience/phar/amlodipine%20besylate.htm