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Premium member Presentation Transcript EVALUATION OF CRUDE DRUG and its formulation BY UV SPECTROSCOPY : EVALUATION OF CRUDE DRUG and its formulation BY UV SPECTROSCOPY PREPARED BY:- VIJAY RADADIYA M.PHARM-II QUALITY ASSURANCE CONTENT:- : CONTENT:- Evaluation of following crude drugs by UV Spectroscopy SENNA SENNA TABLET DIGITOXIN DIGITOXIN TABLET UV SPECTROSCOPY : UV SPECTROSCOPY Ultraviolet Spectroscopy is concerned with the study of absorption of UV radiation which ranges from 200nm-400nm. In UV and Visible spectroscopy only the valence electrons absorb the energy, thereby the molecule undergoes transition from ground state to excited state. This absorption is characteristic and depends on the nature of electrons present. Slide 4: When Radiation is passed through a layer of solution containing an absorbing substance, part of the radiation is absorbed. The magnitute of the absorption is expressed in terms of the Absorbance A. A = abc A = Absorbance a = absorbptivity b = path lenth c = concentration SENNA : SENNA B.S:- Senna Leaf consists of the dried leaflets of Cassia senna (Alexandrian senna ), and C. angustifolia (Tinnevelly senna) belongs to family- Leguminosae. CATEGORY:- Laxative. STANDARDS:- Senna Leaf contains not less than 2.5 per cent of Hydroxyanthracene Glycosides, calculated as Sennoside B ASSAY PROCEDURE:- : ASSAY PROCEDURE:- Accurately weighed 0.15gm of the drug, in fine powder and mix with 50ml water and again weighed the mixture. Place on water bath and heat under reflux condenser for 15 minutes Allow to cool Slide 7: Weight and restore the original weight with water. Centrifuge it. Transfer 20 ml supernant liquid to a 150 ml separating funnel. Slide 8: Add o.1ml HCL Shake well Add CHCl3 at three times in 15 ml quantities. Descard the CHCl3 extract. Add 0.1gm of Sodium bicarbonate and shake for 3 min. Slide 9: Centrifuge the aqueous layer and transfer 10.0 ml of the supernant liquid to a 100ml round bottom flask fitted with a ground glass stopper. Add 20ml of ferric chloride solution and mix well. Heat in a water bath under a reflux condenser for 20 min Add 1 ml HCL and continue heating for 20 minutes with frequently Slide 10: shaking until the precipitate is dissolved. Cool, transfer the mixture to a separating funnel and shake with three quantities, each of 25 ml, of ether. combine the ether extracts and wash with two quantities, each of 15 ml, of water. Slide 11: Dilute the ether extracts to 100.0 ml with ether, evaporate 10.0 ml carefully to dryness and dissolve the residue in 10.0 ml of a 0.5% w/v solution of magnesium acetate in methanol. Measure the absorbance of the resulting solution at the maximum at about 515 nm,using methanol as the blank. Slide 12: Calculate the percentage content of hydroxyanthracene glycosides expressed as Sennoside B taking 240 as the value of A(1%, 1 cm) at the maximum at about 515 nm. SENNA TABLET : SENNA TABLET Senna tablet contain the powdered pericarp of Senna fruit (Alexandrian and Tinnevelly). Senna tablet content of total Sennosides, calculated as Sennoside B NLT 85.00% and NMT 115%. For identification of Senna tablet there are Disintegration and Loss on Drying tests are performed. ASSAY PROCEDURE : ASSAY PROCEDURE Weight and powder 20 tablets of Senna All procedure carryout by taking precaution to protect substance from light. To a quantity of the powder containing 7.5mg of total sennosides add 30 ml of water, weight, heat under a reflux condenser on a water bath for 15 minutes. Slide 15: Allow to cool Weight and restore the original weight with water Centrifuge it Transfer 20 ml of the supernant liquid to a separating funnel and add 0.1 ml of 2 M HCl. Slide 16: Shake with two 15 ml quntities of CHCl3 , allow to separate and discard the CHCl3 layer. Add 0.10gm of sodium bicarbonate and shake for 3 min. Centrifuge and transfer 10 ml of liquid to a round bottom flask fitted with a ground glass neck. Slide 17: Add a mixture of 8 ml of Iron (III) chloride solution and 12 ml of water and mix well. Heat under a reflux condenser on a water bath for 20 min, add 1 ml of HCl and continue heating for a further 20 min, shaking frequently, until the precipitate is dissolved. Allow to cool, transfer the mixture to a separating funnel and extract with three 25 ml quntities of Ether. Slide 18: Wash the combined Ether extracts with two 15 ml water and add sufficient Ether to produce 100 ml. Evaporate 10 ml just to dryness on water bath and dissolve the residue in 10 ml of 1 M KOH, filtering if necessary through a sintered glass filter. Measure the absorbance of the resultant solution without delay at the 500 nm By taking A (1 %, 1 cm)- 200 and at λmax – 500 nm. DIGITOXIN : DIGITOXIN B.S:- DIGITOXIN is a Glycoside obtained from leaf of Digitalis Purpurea belong to Family- scrophulariaceae CATEGORY:- Cardiac Glycoside STANDARDS:- Digitoxin contains NLT 95.0 % and NMT 103.0 % of C41H64O13, calculated with reference to the dried substance. ASSAY PROCEDURE : ASSAY PROCEDURE Weigh accurately about 40 mg of crude drug powder, dissolve in sufficient ethanol (95%) to produce 50.0 ml and dilute 5.0 ml of this solution to 100.0 ml with the same solvent. To 5.0 ml of this solution add 3.0 ml of Alkaline picric acid solution. Slide 21: Allow to stand in subdued light for 30 minutes and measure the absorbance of the resulting solution at the maximum at about 495 nm, using as the blank a mixture of 5.0 ml of ethanol (95%) and 3.0 ml of alkaline picric acid solution. Calculate the content of C41H64O13 from the absorbance obtained by repeating the operation using Digitoxin RS in place of the substance being examined and from the declared content of C41H64O13 in Digitoxin RS DIGITOXIN TABLET : DIGITOXIN TABLET Digitoxin tablet contain NLT 90% and NMT 110% of the stated amount of Digitoxin. It used in treatment of congestive heart failure. Also act as Cardiotonic ASSAY PROCEDURE : ASSAY PROCEDURE Weight and powdered 20 tablets of Digitoxin. Weight accurately and quantity of the powder equivalent to 1.25mg of Digitoxin, add 3 ml of water, swirl to disperse the powder and allow to stand for 10 min. Swirling occasionally Slide 24: Add 25 ml of Glacial Acetic Acid, shake for 1 hr. and filter, discarding the 1st few ml of the filterate. To 4 ml of the filterate add a ml of Dimethyl Sulphoxide, dilute to 25 ml with Xanthydrol Reagent. Mix well and allow to stand in dark for 4 hrs (solution-A) Slide 25: At the same time prepare two further solution in the same manner but using for solution B 4.0 ml of Digitoxin Standard solution and for the solution C 4.0 ml of a mixture of 25 volumes of Glacial Acetic Acid and 3 volumes of water and add 1 ml of Dimethyl Sulphoxide, dilute to 25 ml with Xanthydrol reagent. Measure the absorbance of solution A and B at the maximum at about 550 nm using solution C as blank. Slide 26: Calculate the C14H64O13 form of the absorbance obtained and from the declared content of C14H64O13 in Digitoxin RS REFERENCES:- : REFERENCES:- 1.Indian Pharmacopeia-1996 ,volume I and II, Publsihed by controller of publication, Delhi, Page No.- 2. British Pharmacopeia 2004, Volume III and IV, 4th Edition, Amended by supplements 4.1-4.8 inclusive. Page No.- 3. W.C. Evans, Trease and Evans, “Pharmacognosy”, 5th Edition, Published by Elsevier. Page No.- 45, 75, 289, 391, 4. Kokate C.K.,Purohit A.P., “Pharmacognosy” Nirali prakashan,Page No.-197,174,179,196 Slide 28: THANK YOU You do not have the permission to view this presentation. In order to view it, please contact the author of the presentation.