Synthesis and Antimicrobial Activity Of

METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION OF DIACEREIN AND GLUCOSAMINE IN MARKETED PRODUCTM. Pharm Dissertation Protocol Submitted toRajiv Gandhi University of Health Sciences, Karnataka Bangalore – 560041By Mr. MOMIN MOHAMMAD AKBAR G. Department of Quality AssuranceUnder the Guidance of Dr. CHANDRASHEKHAR NARAJJI M.pharm, Ph.D Asst. Professor Department of Quality AssuranceDepartment of Quality Assurance, Acharya & B.M. Reddy College of Pharmacy, Soldevanahalli, Chikabanavara, Bangalore -902009-20111 RAJIV GANDHI UNIVERSITY OF HEALTH SCIENCES BANGALORE, KARNATAKAANNEXURE – II PROFORMA FOR REGISTRATION OF SUBJECTS FOR DISSERTATION1.0 NAME OF THE CANDIDATE MOMIN MOHAMMAD AKBAR GULAM KASAM AND ADDRESS HOME NO. 6/1093 VACHLI FALI, LILAJPUR , TALUKA: DHOLKA-387810, DIST: AHEMDABAD, STATE: GUJRAT. 2.0 NAME OF THE INSTITUTION ACHARYA & B.M. REDDY COLLEGE OF PHARMACY, SOLDEVANAHALLI, CHIKBANAVARA(POST), BANGALORE -560090. 3.0 COURSE OF STUDY AND M. PHARM SUBJECT QUALITY ASSURANCE 4.0 DATE OF ADDMISION 02th May 20095.0 TITLE OF THE TOPIC:METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION OF DIACEREIN AND GLUCOSAMINE IN MARKETED PRODUCT2 6.0 BRIEF RESUME OF THE INTENDED WORK:6.1:- NEED FOR PRESENT STUDY:Extensive literature survey reveals that several analytical spectrophotometric methods have been reported for the estimation of diacerein and for glucosamine. Development of simple analytical methods for the estimation of drugs combination in single dosage form is inevitable and challenging. One such drug combination of diacerein and glucosamine in pharmaceutical dosage form is used as analgesics and antipyretics.1The present study is to make an attempt to establish sensitive and accurate methods for the estimation of diacerein and glucosamine in pure and pharmaceutical dosage form. Based on the objective the plan of the work is as follows:1. Development of new analytical methods 2. Assay of diacerein and glucosamine tablet 3. Accuracy studies 4. Precision studies 5. Stability studies 6. Recovery studies 7. Ruggedness and robustness 8. Statistical evaluation 9. Limit of detection and Limit of quantization3 6.2 GENERAL DISCUSSION:- Glucosamine1,2 Glucosamine a popular alternative medicine used by consumer for the treatment of osteoarthritis. Glucosamine is also extensively used in veterinary medicine as an unregulated but widely accepted supplement having structural formulaHOOH OHO OH H2N Nomenclature : 3-Amino-6-(hydroxymethyl)oxane-2,4,5-trio Other name : 2-Amino-2-deoxy D-glucose chitosamineMolecular formula : C6H13NO5 Molecular weight : 179.17 gm/mol Category : Analgesic and antipyreticSolubility : Water and alcohol soluble Half life : 70 Hours Excretion : Renal, fecal and lung Functional groups : Hydroxyl, primary amine and ether4Diacerein1,3,4 Diacerein is widely used in the treatment of osteoarthritis. It is used as analgesic and antipyretic having structure formulaO O CH O 3 O O H3COO OHNomenclature : 4,5-diacetyloxy-9,10-dioxo-anthracene-2-carboxylic acid Synonyms : Diacetylrhein, diacerheinMolecular formula : C19H12O8 Molecular weight : 368.294 gm/mol Category : Analgesic and antipyretic Solubility : Soluble in dimethylamine and dimethylsulphoxide Half life : 4-5 Hours Excretion : Renal Functional groups : Ketone, carboxylic acid and ester5 6.3 REVIEW OF LITERATURE: 1. Shao Y et al., reported assay of glucosamine in bulk form and solid dosage formulations. The HPLC separation was achieved by luna amino column (150 mm × 4.6 mm i.d. 5 µm particle size) using a mobile phase of acetonitrile- phosphate buffer (75:25, v/v, pH 7.50) at a flow rate of 1.5 ml min-1 and UV detection at 195 nm.5 2. Zhou J et al., developed method for the determination of glucosamine in raw materials and dietary supplements containing glucosamine sulfate and/or glucosamine hydrochloride by using HPLC and UV with N-(9- fluorenylmethoxycarbonyloxy) succinimide (FMCO-Su) derivatization.6 3. Mahboob N et al., developed high-performance liquid chromatography (HPLC) method for the determination of glucosamine in dosage form. Glucosamine was derivatized by addition of a solution containing orthophthaldialdehyde. The HPLC separation was achieved on a spherimage 80 ODS2 column (250 × 4 mm id, 5 μm particle size) using an isocratic mobile phase containing phosphate buffer- methanol (90:10, v/v, pH 6.50) and methanol-tetrahydrofuran (97:3, v/v) in proportions of 85:15 , followed by fluorescence detection.7 4. Guo ZC et al., investigated UV, IR and 1H-NMR spectral characteristics of complexes which are formed by glucosamine and Fe (II), Zn (II), Co (II), Cu (II) respectively. The UV λmax of the complexes makes obvious violet shift when compared with that of the glucosamine. In IR spectra of the complexes, out-of- plane vibration peak 655 cm-1 of the amino group is lower than that of the glucosamine which is 670 cm-1, and there is also the new absorption peak near 990 cm-1. As for 1H-NMR, the C-3 hydroxy proton and the amino proton of the complexes absorb high field when compared with that of glucosamine, while the shifts of the hydroxy proton on other carbon atoms remain unchanged, so the formation of the nitrogen-metal bond is primarily proved.86 5. Rao J et al., reported stability-indicating HPLC method and validated for diacerein in capsule dosage form. An isocratic separation was achieved using a perfectsil target ODS-3(250×4.6 mm i.d., 5 μm particle size columns with a flow rate of 1 ml/min) and using a UV detector to monitor the eluate at 254 nm. The mobile phase consisted of phosphate buffer:acetonitrile (40:60, v/v) with pH 4.0 adjusted with phosphoric acid.9 6. Ali AH et al., developed high performance liquid chromatographic method for the determination of glucosamine in rat plasma by using isocratic HPLC system consisting of a C18 column, a mobile phase of acetonitrile:water:acetic acid:triethylamine (4.5:95.5:0.1:0.05), a flow rate of 0.9 ml/min and UV detector set at 254 nm.10 7. Liang Z et al., reported selective and specific high performance liquid chromatography method to quantify glucosamine hydrochloride in raw materials, dosage forms and plasma. The mobile phase consisted of methanol: water: acetic acid (10:89.6:0.04) and was pumped at a flow rate of 1.2 ml/min. For the plasma assay, beagle dog plasma was used.11 8. Aldo R et al., worked on sensitive and specific HPLC-ESI-MS/MS method for the direct determination of glucosamine in human plasma has been developed and validated. Plasma samples were analyzed after a simple, one-step protein precipitation, clean-up with trichloroacetic acid using a polymer-based on amino high-performance liquid chromatography (HPLC) column and a water/acetonitrile mobile phase elution gradient, with d-[1-13C] glucosamine as the internal standard. Detection was performed by mass spectrometry, using an electrospray source.12 9. Li Q et al., developed robust capillary electrophoretic method for separate amino saccharides including glucosamine, galactosamine, N-methylglucamine, N-acetyl- glucosamine and amino glucuronic acid. All the aminosaccharides were dansylated fast under microwave irradiation at 385W for 6 min (about 50-fold faster than common methods) and detected via on-line UV adsorption at 214 nm.137 10. Zhongming L et al., developed selective and specific high performance liquid chromatography method to quantify glucosamine hydrochloride in raw materials, dosage form and plasma. Reverse phase chromatography using pre-derivatization with phenylisothiocyanate, and ultraviolet detection (254 nm) was used to quantify the eluate. The mobile phase consisted of methanol:water:acetic acid (10:89.6:0.04).14 11. Yasser SE et al., worked on simple, rapid, selective and specific high performance liquid chromatographic (HPLC) method to quantify glucosamine and its (α-1-4)- d-polymeric form chitosan. The chromatographic separation was achieved using an amino phase column and refractive index (RI) detection. The mobile phase consisted of ACN: water: acetic acid (50:50:0.02) and pH was adjusted to 4.0.15 12. Topagi KS et al., developed two simple UV method for estimation of diacerein and aceclofenac dosage form. Method 1 is absorbance correction method and method 2 is the dual wavelength method.16 13. Tao MH et al., developed and validated for the assay of a liquid chromatography- electrospray ionization mass spectrometry method glucosamine sulfate in human plasma. Chromatographic separation was performed on a C18 column (inertsil ODS-3 150 × 2.1 mm i.d., 5 µm, JP) with a mobile phase gradient consisting of 0.2% acetic acid (aqueous) and methanol at a flow-rate of 0.3 ml/min. MS detection using electrospray ionization (ESI) as an interface was used in single ion monitoring mode to determine positive ions at m/z 297.176.4:- OBJECTIVES OF THE STUDY:In the proposed work, attempts shall be made:  To develop and validate simple, precise, and accurate methods for the simultaneous estimation of diacerein and glucosamine in pharmaceutical dosage formulations by use of instrumental methods like HPLC, UV/Vis spectrometer. To validate the method developed by using various analytical parameters such as accuracy, precision, specificity, robustness, ruggedness, linearity and range.87.0 MATERIALS AND METHODS: HPLC METHOD:High performance liquid chromatography (HPLC) can be used to resolute, identify and quantify the compounds that are present in any sample. This technique can be employed for simultaneous determination of the combination product. The principle involved in this method is differential partition and differential adsorption depending upon the column used.UV/VISIBLE SPECTROPHOTOMETRY:UV/Vis spectroscopy can be employed to identify & quantify the compounds present in most of the samples, present alone or in combination with other drugs. The limitation in this method is that it is less sensitive when compared to HPLC.7.1:- SOURCE OF DATA: The data will be obtained from: 1. JOURNALS:  Analytical Chemicals Acta  Indian Journal of Chemical Technology  Journal of Pharmaceutical and Biomedical Analysis  Indian Journal of Pharmaceutical Sciences  Journal of Chromatography  Journal of Chinese Chemical Society  Biomedical Chromatography  Electrophoresis9 2. RELATED LINK: 1. www.sciencedirect.com 2. www.google.com 3. www.wikipedia.com 4. www.pubmed.com 5. www.cat.inist.com7.2: METHOD OF COLLECTION OF DATA: All experiments shall be carried out in the Department of Quality Assurance, Acharya & B.M. Reddy College of Pharmacy, Bangalore-90. Pure samples of Diacerein and Glucosamine shall be procured from industries involved in the manufacture of these drugs or from suppliers. The HPLC method shall be developed and validated in Department of Quality Assurance lab of Acharya & B.M. Reddy College of Pharmacy, Bangalore-90.7.3: DOES THE STUDY REQUIRE ANY INVESTIGATION OR INTERVENTIONS TO BE CONDUCTED ON THE PATIENTS OR OTHER HUMAN/ANIMALS? IF SO, PLEASE DESCRIBE BRIEFLY.- No –7.4: HAS ETHICAL CLEARANCE BEEN OBTAINED FROM YOUR INSTITUTION IN CASE OF 7.3?- Not Applicable-10 8.0 LIST OF REFERENCES: 1. CIMS-105,Banglore:CPMMedica Indian Private Limited 2009, April; p.182. 2. Glucosamine drug profile [cited 2009 Nov19]. Available at URL:http://en.wikipedia.org/wiki/Glucosamine. 3. Diacerein. drug profile [cited 2009 Nov19]. Available at URL:http://en.wikipedia.org/wiki/Diacerein. 4. Diacerein drug profile [cited 2009 Nov19]. Available at URL:http://www.made- in-china.com/showroom/xahclu/product-detailhqoQzZrHYEVR/China- Diacerein.html. 5. Shao Y, Rama A, Mike M, Uwe K, Stanley L. A stability-indicating HPLC method for the determination of glucosamine in pharmaceutical formulation. J Pharm Biomed Anal 2004;35(3):625-31. 6. Zhou J, Waszkuc T, Mohammed F. Determination of glucosamine in raw materials and dietary supplements containing glucosamine sulfate and/or glucosamine hydrochloride by HPLC with FMOC-Su derivatization. J AOAC Int 2004;87(5):1083-92. 7. Mahboob N, Hadi V, Masood A, Farank G. Development of a simple and sensitive high-performance liquid chromatography method for determination of glucosamine in pharmaceutical formulation. J AOAC Int 2007;90(2):354-7. 8. Guo ZC, Han L, Hu B, Li SN. Spectra characteristics of the complexes of glucosamine and carboxymethyl glucosamine with ferrum(II), zinc(II), cobalt(II) and copper(II). Guang Pu Xue Yu Guang Pu Fen Xi 2002;22(6):963-6. 9. Rao J, Chauhan K, Mahadik KR, Kadam SS. A stability-indicating high performance liquid chromatographic method for the determination of diacerein in capsule. J In Pharma Sci 2009;71(1):24-9. 10. Ali AH, Saeed S, Franco P, Fakhreddin J. High performance liquid chromatographic determination of glucosamine in rat plasma. J Pharma Phamaceut sci 2002;5(2):176-80.11 11. Liang Z, Leslie J, Adebowale A, Ashraf M, Eddington ND. Determination of the nutraceutical, glucosamine hydrochloride, in raw materials, dosage forms and plasma using pre-column derivatization with ultraviolet HPLC. J Pharm Biomed Anal 1999;20(5):807-14. 12. Aldo R, Laura S, Anna B, Massimo G, Marcello L. Development and validation of a sensitive HPLC-ESI-MS/MS method for the direct determination of glucosamine in human plasma. J Chromatogr B 2006;844:119-26. 13. Li Q, Shu FZ, Min Z, Yi C. Capillary electrophoretic determination of glucosamine in osteoarthritis tablets via microwave-accelerated dansylation. J Pharm Biomed Anal 2006;41:1620-4. 14. Zhongming L, James L, Abimbola A, Mohammed A, Natalie DE. Determination of the nutraceutical, glucosamine hydrochloride, in raw materials, dosage forms and plasma using pre-column derivatization with ultraviolet HPLC. J Pharm Biomed Anal 1999;20:807-14. 15. Yasser SE, Ahmed AB. High-performance liquid chromatographic determination of neutraceuticals, glucosamine sulphate and chitosan, in raw materials and dosage forms. Anal Chim Acta 2006;462:125-31. 16. Topagi KS, Sinha PK, Jeswani RM, Damle MC. Simultaneous spectrophotometric determination of aceclofenace in combined pharmaceutical dosage form. Int J Chem Tech Res 2009;1(4):991-5. 17. Tao MH, Lei C, Bei Y, Man XZ, Yun FS, Geng LD. Liquid chromatography with electrospray ionization mass spectrometry method for the assay of glucosamine sulfate in human plasma. Biomed Chromatogr 2005;20(3):251-6.12 9. SIGNATURE OF THE CANDIDATE10. REMARKS OF THE GUIDE11.0 NAME AND DESIGNATION OF:11.1 GUIDE Dr. CHANDRASHEKHAR NARAJJI, Asst. Professor, Department of Quality Assurance, Acharya & B.M. Reddy College of Pharmacy, Soldevanahalli, Bangalore-90.11.2 SIGNATURE11.3 CO-GUIDE NIL11.4 SIGNATURE NIL11.5 HEAD OF THE DEPARTMENT Mr. A. CENDIL KUMAR, Asst. Professor, Department of Quality Assurance, Acharya & B.M. Reddy College of Pharmacy, Soldevanahalli, Chikbanavara(post) Bangalore-90.11.6 SIGNATURE12.0 12.1 REMARKS OF THE PRINCIPAL12.2 NAME OF THE PRINCIPAL Dr. DIVAKAR GOLI Principal, Acharya & B.M. Reddy College of Pharmacy, Soldevanahalli, Chikbanavara(post), Bangalore-90.12.3 SIGNATURE OF THE PRINCIPAL13

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