Pharmaceutics II, LAB MANUAL KINGDOM OF SAUDI ARABIA PRINCE SATTAM BIN ABDULAZIZ COLLEGE OF PHARMACY LABORATORY MANUAL PHARMACEUTICS II PHT-312 LEVEL V Lab Co-ordinator Dr. Shahid Jamil Email:- shahidjamil07@gmail.com 1 Pharmaceutics II, LAB MANUAL Contents Week Experiment, Exercise & Preparation Introduction 1 Introduction of preparation of pharmaceuticals solution, glass ware etc. Aqueous Pharmaceutical Solutions 2 3 1. To prepare and submit 50 ml of concentrated peppermint water BP/ chloroform water BP 0.25 % 2. To prepare and submit 60 ml of gargles. Non aqueous pharmaceutical solution 4 3. To prepare and submit 20 ml of elixirs as non-aqueous preparation. 4. To prepare and submit 50 ml of glycerides by using given formula. Sweet & Viscid Pharmaceutical Solutions 5. To prepare and submit 20 ml of 5 simple syrups by using given formula. Pharmaceutical Emulsions 6. To determine emulsifying agent on the basis of HLB value of surfactant 7. To prepare and submit 20 ml of mineral oil emulsion 8. To prepare and submit 20 ml of 7 castor oil emulsion Pharmaceutical Suspensions and colloids 6 8 9. To prepare and submit 50 ml of barium sulfate suspension. 2 QC/Lab Lab LAB discipline Indiscipline RECORD (5) (-5) (5) Page no Pharmaceutics II, LAB MANUAL Suspension 10. To prepare and submit 50 ml of antacid suspension. 11. To prepare and determine the sedimentation rate of magnesium 9 hydroxide suspension and effect of electrolyte on degree of flocculation. Preparation of lotions 12. To prepare and submit 10 ml of calamine lotion. 13. To prepare and submit 10 ml of scalp lotion. Semisolid dosage form 11 12 13 14. To prepare and submit 10 g of toothpaste. 15. To prepare and submit 10 g of zinc oxide paste. 16. To prepare and submit 10 g of vicks ointment (10%) 17 To prepare and submit 10 g of zinc oxide ointment. Note: All grading should be accompanied by signature of Lab instructor. Note 2: Lab record must be checked on or before next experiment. (Late submission means losing 1 grade/day) Note 3: Final Lab exam (10) + viva/ synopsis/ other activities/ (5) 3 Pharmaceutics II, LAB MANUAL Lab Indiscipline (-5) St Name Attendance Late entry (-1) No lab Lab Dirty Dirty coat Indiscipline Workplace (-1) Glass wares (-1) (-1) (-1) Note: This form is to be kept with Lab instructor 4 Pharmaceutics II, LAB MANUAL INTRODUCTION Solutions Simple solutions (containing soluble substances only) General Method Stage [1] Dissolve the solids in about three quarter of the vehicle; Substances in list A: simply add the material, without previous powdering, to the vehicle in a measure, and stir until dissolved. Substances in list B: finely powder the material in a mortar, add the vehicle, and stir until dissolved. Then transfer the solution to a measure, rinse the mortar with a small quantity of vehicle, and add to the contents of the measure. The term "vehicle" is used to denote the liquid in which the medicinally-active ingredients are dissolved or suspended. The vehicle may be inert (e.g. water), or a flavoring agent (peppermint water), or a preserving and sweetening agent (e.g. chloroform water), or it may have some medical property (e.g. in fusion of senna). Three quarters of the vehicle is selected as a suitable proportion for stage 1, for the following consideration. (a) The volume occupied by the other ingredients will rarely exceed the remaining onequarter, but, if it should, the quantity of vehicle used in stage 1 must be reduced. (b) Solution is accelerated by using as much of the solvent. Stage [2] Examine the solution critically by holding it against the light. If particles of foreign matter are visible, strain the solution through a plug of cotton-wool placed in a funnel, and when the solution has passed through, pour a little of the aqueous vehicle on the wool. Stage [3] Add any liquid ingredients. After measuring each, rinse the vessel used with little of the aqueous vehicle, and add to the contents of the measure. The vehicle used in stage 1 may have been heated to facilitate solution of the solid. In each case the liquid must be thoroughly cooled before the addition of any liquid containing a 5 Pharmaceutics II, LAB MANUAL volatile substance. Further, the succeeding stages 4 and 5 must be completed as quickly as possible, to minimize loss by volatilization from the open measure. Practically, it is preferable to adjust the mixture to volume minus the volume of the volatile liquid, transfer to the bottle, add the volatile liquid, and cap immediately. Stage [4] Add more of the vehicle to produce the prescribed volume. Adjustment to volume should be made in a graduated measure, because of the frequent discrepancy between the supposed and actual capacity of dispensing bottles. The stirrer must, of course, be removed from the measure before adjusting to volume. Stage [5] Transfer the mixture (solution) to the bottle; cork, and then thoroughly polish the bottle to remove finger-marks. Attach the label. Soluble substances A number of water-soluble substances in common use appears in the following lists. Some of these substances are much less than others, but they are administered in smaller doses, or in weaker solutions, so that, as ordinarily prescribed they will dissolve. List [A] a- Substances that are readily dissolved with stirring: Ammonium bicarbonate. Ammonium chloride. Atropine sulfate. Calcium chloride. Chloral hydrate. Citric acid, Dextrose monohydrate. Ephedrine hydrochloride. Hyoscine hydrobromide. Iron ammonium citrate. Phenobarbitone sodium. Phenol. Potassium citrate. Potassium iodide. Potassium Permanganate. Sodium benzoate. Sodium bicarbonate. Sodium bromide. Sodium carbonate. Sodium chloride. Sodium citrate. Sodium iodide. Sodium metabisulphate. Sodium potassium tartrate. 6 Pharmaceutics II, LAB MANUAL Sodium salicylate. Tannic acid. Zinc sulfate. b- Substances that dissolve more readily in warm water. Magnesium sulphate. Phenazone. Sodium acid phosphate. Sodium sulfate. List [B] Substances that do not readily dissolve unless finely powdered in a mortar before the aqueous vehicle are added. Alum. Borax. Boric acid. Calcium lactate Ferrous sulfate. Sodium phosphate. 7 Pharmaceutics II, LAB MANUAL Name of the glass ware used in pharmaceutics (A) Glass rod (B) Beaker (C) Measuring cylinder (graduated) ( D) Conical flask (E) Mortar / pestle (F) Funnel (G) Dispensing bottle (G) Ointment and chemical Spatula 8 (H) Graduated pipettes Pharmaceutics II, LAB MANUAL AQUEOUS PHARAMACEUTICAL SOLUTIONS AROMATIC WATERS: Aromatic waters are medicated waters. They are clear, saturated aqueous solutions of volatile oils. They used as flavoring vehicles in pharmaceuticals and cosmetics or as carminativ e agent. Example: Chloroform water, camphor water, peppermint, orange and rose water. Due to salting out of certain ingredients such as soluble salts the preparations of the formulation having aromatic water showed some problem. Replacement of part of the aromatic water with purified water is the solution of this problem. Storage: Must be stored in airtight light-resistant containers. Method of preparation: Dissolution: these methods are simpler, quicker and more economical as compare to distillation. According to the method recommended in I.P. the corresponding essential oil from which the aromatic water is to be prepared, should be shaken with 500 times its volume of purified water. Shaking is repeated several times during a period of about thirty min utes. The mixture is then set aside overnight and clarifies by filtration. For e.g. chloroform water. Another dissolution method consists of incorporating 2 ml of volatile oil or 2 g suitably comminuted aromatic solid with 15 g of powdered talc or sufficient quantity of kieselghur or pulp filter paper. 1000 ml of purified water is added to this mixture and the resulting slurry is thoroughly agitated several times for about 10 min and filtered. More purified water is passed through the filter paper to make up the volume. Powdered talc, kieselghur pulp filter paper and purified siliceous earth serve two purposes. They act as filter aid and render the product more clear and as distributing agent for aromatic substances. 9 Pharmaceutics II, LAB MANUAL EXPERIMENT NO: 1 AIM: To prepare and submit 50 ml of concentrated peppermint water BP. Apparatus: Beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod. Materials: peppermint oil, alcohol (ethanol), purified water. Formula: Rx Peppermint oil 20 ml Alcohol (90%) 600 ml Purified water q.s 1000 ml Procedure: Peppermint oil is dissolved in alcohol. Sufficient purified water is then added in successive portions, shaking vigorously after each addition. Final volume is then made up with more purified water. However, purified talc or other filtering aid may be added and the mixture shaken occasionally for a few hours and finally filtered. Storage: it should be stored in well closed container, in a cool place. Dose: 0.3 to 1 ml. Theory: main active constituent of peppermint oil are methyl acetate, an ester and free menthol. Formula: Pippermint oil : 1 ml Alcohol (90%) : 30 ml Purified water qs : 50 ml Uses: carminative Dose : 0.3-1 ml Secondary Label: shake well before use Storage : Store in tight closed container , in cool place. Batch No: A-301 Date of Manufacturing: Date of Expiry: Manufactured By: Your name or ID no 28-Sep-11 10 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: Observations & Results: Indication: 11 Pharmaceutics II, LAB MANUAL EXPERIMENT NO: 2 AIM: To prepare and submit 50 ml of chloroform water BP 0.25 %. Apparatus: Beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod. Materials: chloroform, purified water. Formula: Rx Chloroform 2.5 ml Purified water up-to 1000 ml Procedure: Chloroform (0.1 ml) is dissolved by shaking in purified water sufficient to produce 50 ml. Note: Chloroform is slightly soluble (1: 200 at 20º C) in water. Storage: it should be stored in well closed container, in a cool place. Chloroform water should be protected from light. Dose: 15 to 30 ml. Use: vehicle and preservative. 12 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: Observations & Results: Indication: 13 Pharmaceutics II, LAB MANUAL GARGLES: Gargles are aqueous solutions used for treating the pharynx and nasopharynx by forcing air from the lungs through the gargle which is held in the throat. EXPERIMENT NO: 3 AIM: To prepare and submit 60 ml of gargles preparation by using following formula. Apparatus: Beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod. Materials: phenol, menthol, glycerin, boric acid. Formula: Rx Phenol (1%) 1.0 ml Menthol (1%) 0.5 ml Glycerin 15 ml Boric acid solution (1.5%) ad 120 ml Mitte: 60 ml. Sig.: dil. ut dict.(dilute as per direction) Procedure: Menthol is dissolved in 1 ml. of alcohol; with stirring add the phenol and glycerin dissolved in the boric acid solution. A clear solution will formed. 14 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: Observations & Results: Indication: 15 Pharmaceutics II, LAB MANUAL NON AQUEOUS PHARMACEUTICAL SOLUTION ELIXIRS: Elixirs are clear, pleasantly flavored, sweetened hydro- alcoholic liquids intended for oral use. They are used as flavors and vehicles for drug substances and when such substances are incorporated into the specified solvents, they are classified as medicated elixirs. The main ingredients in the elixir are ethanol and water but glycerin, sorbitol and propylene glycol, flavoring agents, preservatives and syrups are often used in the preparation of the final products. The alcoholic content of elixirs varies greatly from elixirs, only a small quantity to those that contains a considerable portion as a necessary aid to solubility. For example; Aromatic Elixir USP contains 21 – 23% ethanol; Compound benzaldehyde elixir NF contains 3 - 5% ethanol. Elixirs may also contain glycerin and syrup. These may be added to increase the solubility of the medicinal agent or for sweetening purpose. Some elixirs contain propylene glycol. This solvent is a satisfactory substitute for both glycerin and ethanol. Sucrose increase viscosity and decreases the solubilizing properties of water and so must be added after primary solution has been carried out. A high alcoholic content is maintained during preparation by adding the aqueous phase to the alcoholic solution. Elixirs should always be brilliantly clear. They may be strained or filtered and if necessary, subjected to the clarifying action of purified talc or siliceous earth. 16 Pharmaceutics II, LAB MANUAL EXPERIMENT NO: 4 AIM: To prepare and submit 10 ml of elixirs as non-aqueous preparation. Apparatus: Beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod. Materials: compound orange spirit, alcohol, glycerin, sucrose, purified water. Formula: Rx Compound orange spirit 10 ml. Alcohol 100 ml. Glycerin Sucrose Purified water, q.s. 200 ml. 320 g. 1000 ml. Ft.: elix. Procedure: 1) Take three quarter of water, warm on hot plate dissolve the sucrose into this warm water. 2) Mix the alcohol, glycerin, to it. 3) Filter the solvent mixture through a hard filter paper, returning, if necessary, the first portions of the filtrate until it passes through clear. 4) Add enough of vehicles make the volume upto10 ml. Note (Alcohol content: 8 - 10 %) 17 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: Observations & Results: Indication: 18 Pharmaceutics II, LAB MANUAL GLYCERITES: Glycerites are solutions or mixtures of medicinal substances are not less than 50% by wt glycerin. Most of glycerites are extremely viscous and some of them are of a jelly-like consistency. The advantages of glycerin in these preparations are: 1) A valuable solvent, being composed of a polar and non-polar groups, it has a wide range of solvent power. 2) Its sweet taste. 3) Has a preservative action. 4) Stable. 5) Miscible with water and alcohol, thus liquid glycerites can serve as stoke solution which may be diluted with water or alcohol. EXPERIMENT NO: 5 AIM: To prepare and submit 50 ml of scar phenol ear drops by using following formula. Apparatus: Beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod. Materials: phenol, glycerin. (A) To prepare 50 ml of Phenol Glycerin BPC Phenol Glycerin BPC Rx Phenol 160 g Glycerin 840 g Density: Phenol = 1.07 g/cm3, Glycerin = 1.261 g/cm3 Procedure: Dissolve phenol in glycerin (B) Scar Phenol ear drops BPC Rx Phenol glycerin 15 ml Glycerin up-to 50 ml Ft.: liq. Sig: gtt. au 19 Pharmaceutics II, LAB MANUAL Procedure: Take the measured amount of phenol glycerin and diluted with sufficient amount of glycerin up to 50 ml. Uses: used as antiseptic Ear drops Storage: store in tightly closed container Dose: 2-3 drops, three times in a day to each ear. Theory: Precautions The ear should not be damp. Water should not be added to this preparation. It reacts with phenol to produce a preparation which is caustic, and consequently, damaging the area of application. 20 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: Observations & Results: Indication: 21 Pharmaceutics II, LAB MANUAL SWEET & VISCID PHARMACEUTICAL SOLUTIONS SYRUPS: Syrups are concentrated solutions of a sugar such as sucrose in water or other aqueous liquids. When purified water alone is used in making the solution of sucrose, the preparation is known as syrup, or simple syrup. In addition to sucrose, certain other polyols, such as glycerin or sorbitol, may be added to retard crystallization of sucrose or to increase the solubility of added ingredients. When the aqueous preparation contains some added medicinal substance, the syrup is called medicated syrup. Flavored syrup is one which is usually not medicated, but which contains various aromatic or pleasantly flavored substances and is intended to be used as a vehicle or a flavor for prescriptions. EXPERIMENT NO: 6 AIM: To prepare and submit 10 ml of simple syrups B.P, by using following formulas. Apparatus: Beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod. Materials: sucrose, water. Formula: Rx Sucrose 85 g Water to 1000 ml Ft: Simple syr. Mitte: 20 ml. Procedure: Take the three quarter of vehicle and warm it on hot plate. Then dissolved the calculated amount of sucrose. Finally make up the volume by same vehicle. Uses: used as simple syrups and vehicle. Storage: store in tightly closed container 22 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: Observations & Results: Indication: 23 Pharmaceutics II, LAB MANUAL EMULSIONS An emulsion consists of two phases, one of which is finely divided and dispersed in the continuous phase. The system is stabilized by the presence of a third substance known as the emulsifying agent. Types of Emulsion 1. Oil-in-water emulsions O/ W: The internal phase/dispersed phase is oil and external/ continuous phase is water. 2. water-in-Oil emulsions W/O: The internal phase/dispersed phase is water and external/ continuous phase is oil. Methods for Preparing Emulsions: One of the following general methods is employed: I. The Dry Gum Method II. The Wet Gum Method The Dry Gum Method/wet gum method In this method, a primary emulsion is made from certain proportion of oil, water and gum. Type of method is depending on the order of addition of gum, water and oil. When a stable primary emulsion has been obtained, it may be freely diluted with more of the continuous phase (water in o/w emulsions). Any salts or flavoring agents are added in dilute solutions just before adjusting the volume. The Quantities for primary emulsions A. Fixed oil, e.g., almond, castor, arachis and cod liver oil. Oil : water : gum 4 : 2 : 1 B. Volatile oil, e.g., turpentine, cinnamon and peppermint oil. Oil : water : gum 2 : 2 : 1 C. Mineral oil (liquid paraffin). Oil : water : gum 3 : 2 : 1 24 Pharmaceutics II, LAB MANUAL HLB determination An arbitrary scale was devised by the scientist Griffin to serve as a measure of the hydrophilic – lipophilic balance (HLB) of surfactant. By means of this scale it is possible to assign a HLB range of optimum efficiency for each class of surfactant. The hydrophilic surfactant has the HLB value 10-18, and lipophilic surfactant have the HLB value less than 10. Required HLB value: It has be found that certain emulsifying agents of a given HLB value appear to have the best effect when used in combination with particular oil phase. It has given rise to the concept of Required HLB for given oil or oil combination, which is defined as the HLB value that is required to prepare a stable emulsion of particular type. Thus for a given oil, the RHLB of preparing a stable O/W emulsion can be different from that required to prepare a stable W/O emulsion. 25 Pharmaceutics II, LAB MANUAL 26 Pharmaceutics II, LAB MANUAL Experiment No 7 AIM: To determine emulsifying agent on the basis of HLB value of surfactant and prepare and submit 100 gm mineral oil emulsion. Apparatus: Mortar pestle, beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod. Materials: Tween 80, Span 80, liquid paraffin, wool fat. HLB Determination The following example illustrates the use of HLB to determine the proportions of two surfactants: Polysorbate 80 with HLB = 15 Sorbitan monoolate with HLB = 4.3 Which are used as emulsifying agent in the following o/w and w/o systems: Mineral oil Rx Liquid paraffin (required HLB=12) 30 gm Wool fat (required HLB=10) 5 gm Emulsifying agent Water to 5 gm 100 gm Fiat: emuls Mitte: 100 g Uses: used as lubricant laxative Sig: take on empty stomach, at least 1 hr before and 2 hr after meal Dose: 1 or 2 spoonful and add small amount of water (less than 30 ml) Calculation: - For O/W emulsion Liquid paraffin (required HLB=12) Wool fat (required HLB=10) 27 Pharmaceutics II, LAB MANUAL . ........... Calculation: - For W/O emulsion Liquid paraffin (required HLB=5) Wool fat (required HLB=8) ............ 28 Pharmaceutics II, LAB MANUAL Note: Density of given liquids Liquid Paraffin: 0.83-0.86 gm/ml Tween 80: 1.06 Span: 0.986 Preparation of mineral oil emulsion: 1) Ration for the primary emulsion of mineral oil is: oil : water : gum 3 : 2:1 2) Calculated formula of given formula 15: 10 : 5 3) Either the dry gum method or the wet gum method can be used, but the former is more suitable. 4) In this formulation we are taking two oils and two emulsifying agents As per our previous calculation. We calculate all values. Procedure: a) Select a sample-sized mortar and a suitable pestle. b) Weigh the accurate amount of wool fat (2.14 g) in beaker and melt it on hot plate. c) Place in the mortar 12.85 gm (15.11 ml) of liquid paraffin then add melted wool fat to it. d) Measure 3.4 5 gm (3.3 ml) of tween 80 and 1.55 g (1.57 ml) of span 80 and add to it into above liquid. 29 Pharmaceutics II, LAB MANUAL e) Triturate the oil phase and EA together for a few seconds. f) Measure exactly 10 ml of water in another measure. g) Begin to triturate the oil and, EA again using whipping motion, but not a grinding action. While triturating, add water slowly. h) As the water reaches the oil-EA mixture, increase the rate of trituration, taking care to maintain the whipping motion and work in one direction only. i) Continue trituration till the primary emulsion is formed. This is when the mixture becomes white in colour and clicking sound is heard. j) Continue to triturate for a little longer before attempting to dilute. k) Measure small amount of water and add them drop wise, with continuous trituration, to the primary emulsion and then dilute with remaining amount of water and transfer to a measure. l) Rinse the mortar with more water and adjust the volume. 30 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: 31 Pharmaceutics II, LAB MANUAL Observations & Results: Indication: 32 Pharmaceutics II, LAB MANUAL Experiment No 8 AIM: To prepare and submit 40 ml of castor oil. Apparatus: Mortar pestle, beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod Materials: castor oil, gum acacia, water. Fixed Oil Formula: Castor Oil Emulsion Rx Castor oil 16 ml GUM acacia Q.S. Water 80 ml Fiat: emuls Sig. Stat Uses: Castor oil is administered orally as a purgative. Castor oil is a fixed oil. Therefore, the primary emulsion Formula used is: Oil: water: gum 4: 2 :1 Either the dry gum method or the wet gum method can be used, but the former is more suitable. Method of preparation 1. Select a sample-sized mortar and a suitable pestle. 2. Place in the mortar 2 g. acacia (very finely pulverized). 3. Measure 8 ml of oil in a dry measure and pour on the gum allowing some time for the measure to drain. 4. Triturate the oil and gum together for a few seconds. 5. Measure exactly 4 ml of water in another measure. 33 Pharmaceutics II, LAB MANUAL 6. Begin to triturate the oil and, gum again using whipping motion, but not a grinding action. While triturating, add water all at once. 7. As the water reaches the oil-gum mixture, increase the rate of trituration, taking care to maintain the whipping motion and work in one direction only. 8. Continue trituration till the primary emulsion is formed. This is when the mixture becomes white in colour and cracking sound is heard. 9. Continue to triturate for a little longer before attempting to dilute. 10. Measure small amount of water and add them drop wise, with continuous trituration, to the primary emulsion and then dilute with remaining amount of water and transfer to a measure. 11. Rinse the mortar with more water and adjust the volume. Castor oil emulsion USP (40 ml) Formula: Castor oil : 6.4 ml gum acacia : 1.6 g Water : 28.8 ml Uses: used as purgative Direction for Use: immediately Dose : swallow in one time Secondary Label: shake well before use Storage : Store in tight closed Container. Batch No: Date of Manufacturing: Date of Expiry: Manufactured By: 34 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: Observations & Results: Indication: 35 Pharmaceutics II, LAB MANUAL Suspension Pharmaceutical suspension is a biphasic system composed of finally divided insoluble solid material suspended in liquid medium. The average size of suspended particles ranges from 0.5 µm to 5 µm in most of the pharmaceutical suspensions. Suspensions essentially facilitate the administration of insoluble and often distasteful substances in a form which is pleasant in taste. Properties of good suspensions 1. Upon shaking the particles should be in suspension for a long time enough for the removal of the correct dose. 2. The sediment produced on standing should be easily redispersed. 3. It is easily removed from the container. 4. They should not cake on settling. 5. Their taste should be acceptable to the patient. Factors affecting the settling in Suspension While it is seldom possible to prevent settling completely over a prolonged period of time, it is necessary to consider the factors which influence the velocity of sedimentation. The velocity of sedimentation is expressed by stokes law V = 2r2 (Ps - Po) g 9η Where V : The terminal velocity in cm/sec. r :The radius of the particles in cm . Ps: The density of the dispersed phase. PO: The density of the dispersion medium g : The acceleration due to gravity η : viscosity of !he dispersion medium in poise 36 Pharmaceutics II, LAB MANUAL Sedimentation volume: Sedimentation volume is the most important parameter in the evaluation of suspension stability. Sedimentation volume F is the ratio of ultimate height of the sediment (Hu, height after sedimentation) to the initial height (Ho) of the total suspension. Sedimentation volume or rate (F) = ultimate height of sediment (Hu) Initial height of suspension (Ho) Sedimentation volume can be plotted against time abscissa and the resultant curve indicates the sedimentation pattern at storage. 37 Pharmaceutics II, LAB MANUAL Experiment No 9 AIM: To prepare and submit 50 ml barium sulfate suspension. Apparatus: Mortar pestle, beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod. Materials/formula Barium sulfate Suspension Rx Barium sulfate 350.0 g Methyl cellulose (2%) 20.0 g Tween 80, (1%) solution 60.0ml Flavor 5.0 ml Saccharin sodium 0.5 g Sorbitol solution (70%) Purified water to 150.0 ml 1000.0 ml Fiat (let it be made): Draught (large amount swallow in one time) Mitte (send): 50 ml Sig: Stat. (immediately) Procedure: 1. Prepare the methyl cellulose solution by adding small amount of normal water subsequently. 2. Wet the barium sulfate using Tween 80. 3. Add methyl cellulose solution in subsequent amount and triturate well. 4. Dissolve the flavor and saccharin in sorbitol solution and pour into the suspension. 5. Finally add purified water and complete to volume. Uses: It is used as media, during X-ray examination. Dose: whole amount in one time. Storage: store in tight closed container. Secondary label (auxiliary): shake well before use 38 Pharmaceutics II, LAB MANUAL 39 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: Observations & Results: Indication: 40 Pharmaceutics II, LAB MANUAL Experiment No 10 AIM: To prepare and submit 30 ml of antacid Suspension. Apparatus: Mortar pestle, beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod Materials/ formula Rx Magnesium sulphate 5.0 g. Light magnesium carbonate 1.0 g. Peppermint water to 15.0 ml. Fiat: mist. mitte x doses Sig.: 30 ml. o.m. (omn man) (every morning) Procedure: (1) Finally powder magnesium sulphate then mix well with light magnesium carbonate. (2) Measure about three-quarter of the peppermint water, pour a portion of it into the mortar containing the powder and triturate to form a smooth cream; then gradually add the remainder of the vehicle measured out. (3) Examine the contents of the mortar and if particles of foreign matter are visible, spread a piece of muslin over the mouth of the measure, and pour the content, of the mortar through it. (4) Rinse the mortar with a little of the vehicle, and then pass the liquid through the muslin. (3) Finally make up the volume Uses: Laxative and antacid in case of liver cirrhosis. Dose: 30 ml. Storage: store in well closed container Secondary (auxiliary) label: shake well before use. 41 Pharmaceutics II, LAB MANUAL 42 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: Observations & Results: Indication: 43 Pharmaceutics II, LAB MANUAL Experiment No: 11 Determination of Sedimentation rate AIM: To prepare and determine the of sedimentation rate of magnesium hydroxide suspension and effect of electrolyte on degree of flocculation. Apparatus: Mortar pestle, beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod Materials: magnesium carbonate, sodium hydroxide, sodium chloride, sodium carbonate, sodium sulfate, calcium carbonate, distilled water. Procedure: (1) Take five measuring cylinders (50 ml.), transfer 1 g, magnesium carbonate to each one. (2) Add 45 ml. of each of the following electrolytes H2O, N/10 NaCI, N/10Na2CO3 , N/10 Na2SO4, and N/10 Ca2CO3 (3) To each cylinder add 5 ml. N/10 NaOH and mix well. (4) Leave without disturbance and observe the sedimentation of the particles. (5) Measure the total height (initial height Ho) of each mixture in cm, and Then take the 3-4 reading after 5 min interval that is (Hu, ultimate height). (6) Plot the ratio of sedimentation (F) on Y-axis vs. time at X axis. (7) Calculate the velocity (sedimentation rate) by finding the slope x Molecular weight of following compounds Sodium hydroxide (NaOH) = 39.99 g/mole Sodium Chloride (NaCI) = 58.44 g/mole Sodium sulfate (Na2SO4) = 142.04g/mole Sodium carbonate (Na2CO3)= 105.9 g/mole Calcium carbonate (CaCO3)= 100.08 g/mole 44 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Calculations: 45 Pharmaceutics II, LAB MANUAL Observations & Results: Observation table for water S.N Time (min) Hu (cm) 1 0 0 2 5 3 10 4 15 5 20 6 25 Ho (cm) Hu/Ho Ho (cm) Hu/Ho Ho (cm) Hu/Ho Observation table for sodium chloride S.N Time (min) Hu (cm) 1 0 0 2 5 3 10 4 15 5 20 6 25 Observation table for sodium sulfate S.N Time (min) Hu (cm) 1 0 0 2 5 3 10 4 15 5 20 6 25 46 Pharmaceutics II, LAB MANUAL Observation table for sodium carbonate S.N Time (min) Hu (cm) 1 0 0 2 5 3 10 4 15 5 20 6 25 Ho (cm) Hu/Ho Ho (cm) Hu/Ho Observation table for calcium carbonate S.N Time (min) Hu (cm) 1 0 0 2 5 3 10 4 15 5 20 6 25 47 Pharmaceutics II, LAB MANUAL Sedimentation rate curve 48 Pharmaceutics II, LAB MANUAL LOTIONS Lotions are dilute aqueous solutions or suspensions meant for external application to the body. They may be applied to the skin, hair or eyes. They are applied without friction. They may contain: Humectants ; to retain moisture on the skin after application Alcohol ; which evaporates quickly causes a cooling effect and leaving the skin dry. Experiment No 12 AIM: To prepare and submit 10 ml of calamine lotion Apparatus: Mortar pestle, beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod Materials/formula: Rx Calamine 8 g. Zinc oxide 8 g. Glycerin 6 ml. Lime water to 100 ml. Fiat: lotion (to make lotions) Mitte: 10 ml Sig. M.D.U. (More Dicto Utendus) ( to be used as directed) Procedure: I. M i x calamine and zinc oxide together in a mortar till a homogenous powder is obtained. 2. Pour glycerin and triturate to form a homogeneous paste. 3. Add a small portion of lime water and continue trituration till a very smooth levigate is obtained. 4. Dilute the smooth levigate with small portion of calcium hydroxide solution (lime water), then 49 Pharmaceutics II, LAB MANUAL with large portion following by trituration after each addition till attaining the final volume. Uses: Soothing and protective in cases of skin irritation and dermatitis. Lime water: Saturated calcium hydroxide solution (1.5g/L at 25ºC sparsely soluble). 50 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: Observations & Results: Indication: 51 Pharmaceutics II, LAB MANUAL Experiment No 13 AIM: To prepare and submit 10 ml of scalp lotion. Apparatus: Mortar pestle, beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod. Materials/formula: scalp lotion Rx Resorcinol 2.00 g Salicylic acid 2.00 g Sodium metabisulphite 0.01g Glycerin 2.00 ml Alcohol 50% to 100.00 ml Fiat: Lot Mitte: 50 ml Sig. M.D.U. Method of preparation 1) Dissolve resorcinol, salicylic acid and sodium metabisulphite in 2/3 the vehicle, 2) Then add glycerin and adjust to volume with alcohol 50%. Uses: Rubefacient for the scalp and to treat dandruff. 52 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: Observations & Results: Indication: 53 Pharmaceutics II, LAB MANUAL SEMISOLID DOSAGE FORMS Semisolid dosage forms: These are dermatological products of semisolid consistency and applied to skin for therapeutic or protective action or cosmetic function Types of conventional semisolid dosage forms: 1. Ointments 2. Creams 3. Pastes 4. Gels 5. Poultices 6. Plasters 7. Rigid foam Paste: Pastes are the semi-solid dosage forms that contain one or more drug substances incorporated in a base with large proportions of finely dispersed solids, are intended for external application to skin, but very thick and stiff. Tooth paste: Toothpaste is a paste or gel dentifrice used with a toothbrush as an accessory to clean and maintain the aesthetics and health of teeth. Toothpaste is used to promote oral hygiene: it serves as an abrasive that aids in removing the dental plaque and food from the teeth, assists in suppressing halitosis, and delivers active ingredients such as fluoride or xylitol to help prevent tooth and gum disease (gingivitis).[1] Most of the cleaning is achieved by the mechanical action of the toothbrush, and not by the toothpaste. Salt and Baking soda are among materials that can be substituted for commercial toothpaste. Toothpaste is not intended to be swallowed. Levigation Levigation is the process of grinding an insoluble substance to a fine powder, while wet. The material is introduced into the mill together with water, in which the powdered substance remains suspended, and flows from the mill as a turbid liquid or thin paste, according to the amount of water employed. 54 Pharmaceutics II, LAB MANUAL Experiment 14 Aim: To prepare and submit 20 g of tooth paste. Apparatus: Mortar pestle, beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod Materials/formula: Tooth paste: Rx Precipitated chalk (calcium carbonate) 57 Sod Lauryl1504 1.0 Glycerin 21 Gum Tragacanth 1.5 Water qs 20 Send: 20 g g g g g gm Method of preparation; 1) Triturate Precipitated chalk, Sod. Lauryl and Gum in a mortar and mix gradually with litigation. 2) Then add Glycerin to (1) with levigation, until past is formed, add amount of water according to consistency. Uses: use for dentifrices. Packaging and Storage : Fill on Plastic or glass wide mouthed container and collapsible tubes, store at temperature not more than 25 °C. Label : For External use only 55 Pharmaceutics II, LAB MANUAL 56 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: Observations & Results: Indication: 57 Pharmaceutics II, LAB MANUAL Experiment 15 Aim: To prepare and submit 10 g of zinc oxide paste. Apparatus: Porcelain dish, water bath, Mortar pestle, beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod Materials/formula: Rx Zinc oxide 25 gm Starch 25 gm Vaseline to 100 gm Send 10 gm Method of preparation; 2) Melt the Vaseline on water bath to 70ºC 1) Incorporate Zinc oxide and starch to the melted Vaseline with continuous stirring until cold. Uses: As protective. Packaging and Storage : Fill on Plastic or glass wide mouthed container and collapsible tubes, store at temperature not more than 25 °C. Label : For external use only 58 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: Observations & Results: Indication: 59 Pharmaceutics II, LAB MANUAL OINTMENTS: Ointments are semisolid greasy preparations for application to the skin, rectum, nasal mucosal. The base is usually anhydrous and contain the medicament in solution or suspension. Water No: The water number is the largest amount of water in gm that Gm of an ointment base or fat will hold at normal temperature( 20°). Most oleaginous bases can become absorption bases by the addition of an ingredient or ingredients that increase the water number of the oleaginous base. Oleaginous Ointment Bases: Experiment 16 Aim: To prepare and submit 10 g of Vicks ointment. Apparatus: Porcelain dish, water bath, Mortar pestle, beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod Materials/formula: Rx Methyl Salicylate 10ml Menthol 0.22g White Soft Paraffin qs100g Method of Preparation: 1) Accurately measure 10 ml of Methyl Salicylate , 0.22g of Menthol and 90 g of White Soft Paraffin . 2) Then melt white soft paraffin over a water bath , and remove to cool to 25°C. 3) Dissolve menthol in Methyl Salicylate and mix well with the melted white soft paraffin , let it be cooled , mix well in the same direction to become homogenous mixture . 4) Then pass this preparation in the triple Roller mill , two times or more till you get a homogenous ointment . Uses : Is used in Musculoskeletal , joint & soft – tissue disorders &for minor peripheral vascular disorders 60 Pharmaceutics II, LAB MANUAL such as chilblains . It can be used ads inhalation for symptomatic relief of upper respiratory – tract disorders . Doses : Apply to Affected area three times daily . Packaging and Storage : Fill on Plastic Wide mouthed container or ointment tubes, and store at temperature not more than 25 °C . Stability : It is stable for three month Label : For External use only . Protect from light . 61 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: Observations & Results: Indication: 62 Pharmaceutics II, LAB MANUAL Experiment 17 Aim: To prepare and submit 10 g of Zinc oxide ointment. Apparatus: Porcelain dish, water bath, Mortar pestle, beaker (250 ml), measuring cylinder (10 ml. 50 ml), Spatula and glass rod Materials/formual Rx Zinc Oxide 20 g Paraffin Oil 15 g White Soft Paraffin as 100 g Method of preparation: 1) Accurately weigh 20 g of Zink Oxide, 15 g of Paraffin oil and 70 g of White Soft Paraffin. 2) Triturate the Zink Oxide to make fine powder 3) Melt the White Soft Paraffin over water bath, then allow cooling to about 30 °C . 4) Dilute Zinc oxide with paraffin oil with mixing till you get a homogenous preparation , and to them add Soft paraffin with mixing again to get a homogenous preparation . 5) Pass this preparation over triple Roller mill to get homogenous ointment . Uses: used as suns cream, for treatment eczema, slight excoriations. 10% can be used to prevent diaper rash and protect chafed skin due to diaper rash & helps seal out wetness. Doses: For diaper rash : Apply each diaper change , especially at bed time . For eczema and slight excoriations: Apply affected area twice or three times daily . As sun cream apply the skin half an hour before exposure to sun light . Packaging and Storage : Fill on Plastic Wide mouthed container or ointment tubes , and store at temperature not more than 25 °C . Stability : It is stable for three month Label :For External use only . Protect from light . 63 Pharmaceutics II, LAB MANUAL Practical Lab Report Name of Experiment: Date: AIM: Ingredient used and their function: Calculations: Observations & Results: Indication: 64 Pharmaceutics II, LAB MANUAL 65