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By, SUNDARARAMAN S Department of Pharmaceutical Analysis :

By, SUNDARARAMAN S Department of Pharmaceutical Analysis HAIR CARE PRODUCTS & SKIN CARE PRODUCTS 1 S.B.COLLEGE OF PHARMACY,SIVAKASI

INTRODUCTION:

INTRODUCTION THE PRODUCTS WHICH ARE INTENDED TO PROMOTE CERTAIN FAVOURABLE CONDITIONS OF HAIR AND TO REDUCE OR ELIMINATE PROPERTIES OF HAIR WHICH ARE REGARDED AS UNDESIRABLE ARE CALLED AS HAIR CARE PRODUCTS Hair care products include shampoos ,hair creams, conditioners, hair oils, hair tonics. It may be classified into 2 groups Those with work by purely physical mechanisms(shampoos, hair sprays) Those with brings about chemical changes in hair(waving, sting preparations, permanent dyes) 2 S.B.COLLEGE OF PHARMACY,SIVAKASI

SHAMPOO:

SHAMPOO Shampoo is a preparation meant for cleaning hair of dust, dirt, and also to impart luster and gloss to hair. Ph=5-9 CLASSIFICATION: BASED ON APPEARANCE : clear liquid, liquid creams, clear gels, paste, powder, dry. BASED ON FUNCTIONALITY: conditioning, therapeutic,anti-dandruff,mild(baby),acid-balance shampoos. 3 S.B.COLLEGE OF PHARMACY,SIVAKASI

INGREDIENTS:

INGREDIENTS DETERGENTS: sodium lauryl sulphate,sodium lauryl sarcosinate. FOAM BOOSTERS AND STABILIZERS : amide oxides, ethanol amides. CONDITIONINGAGENTS/EMMOLIENS : glycol esters,lanolin,fatty alcohols. VISCOSITY MODIFIERS/THICKENING AGENTS: methyl cellulose, ethyl cellulose 4 S.B.COLLEGE OF PHARMACY,SIVAKASI

Slide 5:

OPACIFIERS/CLARIFYING AGENTS : higher fatty alcohols,di glyceral stearates, HYDROTROPES: alcohols,glycols,sodium benzoate. PRESERVATIVES : methyl parabens, propyl parabens. SEQUESTERING AGENTS : sodium salts of EDTA,sodium poly phosphates. ANTI- DANDRUFF SUBSTANCES : selenium sulphide, selenium disulphide. 5 S.B.COLLEGE OF PHARMACY,SIVAKASI

REQUIREMENTS FOR SHAMPOOS:

REQUIREMENTS FOR SHAMPOOS S.NO CHARACTERSTICS REQUIREMENTS 1 Total fatty matter,% by mass,minimum 15.0 2 Matter insoluable in alcohol,% by mass.maximum 2.0 3 Foam height for 2%soln,minimum 150mm 4 Free caustic alkali(as KOH)%by mass,maximum 0.01 6 S.B.COLLEGE OF PHARMACY,SIVAKASI

EVALUATION OF SHAMPOO:

EVALUATION OF SHAMPOO Determination of foam height: preparation of sample solution: Add 500ml of water to 10g of shampoo solution while stirring in such a manner until misicibility of shampoo with water is complete. Age the soln at a temperature of 30±2ºC for a total period of 30 mts counting the time when the shampoo is first added to water 7 S.B.COLLEGE OF PHARMACY,SIVAKASI

Slide 8:

PROCEDURE: When shampoo soln aging,circulate water at 30±2ºC through water jacket of reciever,rinse the walls. At the completion of aging period close the stop cock at the bottom of reciever,rinse walls with 50ml of soln using pipette Fill pipette with soln to 200ml mark immediately place it in position at thetop of reciever and open the stop cock. When all the soln has run out of the pipette,start stop watch , take a reading of foam height and has taken second reading at the end of 5mts. 8 S.B.COLLEGE OF PHARMACY,SIVAKASI

Slide 9:

Take the reading by measuring the foam column at highest average height to which the rim of foam has reached. The foam height of 2% shampoo soln shall not be less than 150mm 9 S.B.COLLEGE OF PHARMACY,SIVAKASI

Slide 10:

DETERMINATION OF FREE CAUSTIC ALKALI: Ethanol method: Weigh 2-10g of sample, add boiled ethanol freshly, digest until soap is dissolved. Filter the content through, dried gooch/sintered glass crucible(protecting soln from carbon di oxide &acid fumes ,covering with watch glass) Wash with hot ethanol still neutral to phenolphthalein, heat filtrate to boiling Add 0.5ml of phenolphthalein & titrate with standard sulphuric acid /Hcl 10 S.B.COLLEGE OF PHARMACY,SIVAKASI

Slide 11:

Barium chloride method: 10g of sample+100ml ethanol,insert a cork provided with long tube to act as reflux condensor,immerse –boiling water bath ,shake soap dissolves 5ml of barium chloride soln(to eliminate carbonates)+phenolphthalein indicator. Titrate with standard sulphuric acid /Hcl . Free caustic alkali= V=vol. in ml std hcl/sulphuric acid N= normality of std hcl / sulphuric acid M= mass of material taken for test. 4.71VN/M 11 S.B.COLLEGE OF PHARMACY,SIVAKASI

Slide 12:

Matter insoluble in alcohol: 2-10g sample+200ml freshly boiled ethanol digest until soap dissolves Filter into a filter flask through a tared,dried&counter poised filter paper til neutral to phenolphthalein ,through tared&dried gooch sintered glass crucible with suction ,protecting soln from carbondi oxide& acid fumes by covering with watch glass. Wash several times with hot ethyl alcohol to remove all alcohol soluble. Dry the filter paper crucible with the residue at 100±2ºC for 3hrs 7 cool .weigh total insoluble in alcohol. 12 S.B.COLLEGE OF PHARMACY,SIVAKASI

Slide 13:

Matter insoluble in alcohol % by mass = M-mass in g of matter insoluble in alcohol m -mass in g material taken for test Determination of total fatty matter: 10g sample+100ml ethanol,insert a cork provided with long tube to act as a reflux condenser& immerse into boiling water bath, shaking till soap dissolves Titrate with alcoholic soln with std NaoH soln. Free fatty acid as oleic acid,% by mass= 100m/M 28.25V1N1/M 13 S.B.COLLEGE OF PHARMACY,SIVAKASI

Slide 14:

Determination of pH: At a temperature of 27ºC pH is determined, for liquid shampoo, read pH directly from the sample in the form of powder or paste, mix 1g sample with 9ml of water and determine the pH. 14 S.B.COLLEGE OF PHARMACY,SIVAKASI

Hair creams and hair oils :

Hair creams and hair oils Hair creams and oils intended to provide to the hair good grooming,lustre without greasiness, protection from wind, rain, heat and some degree of hair conditioning TYPES: Based on vegetable oil emulsion Based on mineral oil emulsion Based on vegetable-mineral oil emulsion Based on any above combination with fatty acids or its esters. 15 S.B.COLLEGE OF PHARMACY,SIVAKASI

Methods to test hair oil and creams:

Methods to test hair oil and creams Microbiological examination : Melt sufficient number of nutrient agar tubes and sabouraud agar tubes in water bath and transfer while hot into aconstant temperature maintained at 48±2ºC 1g of sample asepticaly to conical flask+50ml dil phosphate buffer at pH7.2. shake Pipette out 1ml into 3 sterile petridishes,pour melted ,cooled(at 45ºC) medium into it & rotate the plates to mix thoroughly Incubate plates at 32ºC for 72 hrs in inverted position. Determine avg no. of colonies on medium plates and multiply by 30,dilution factor (no. of micro organisms per gram of sample ).ISI DOES NOT PERMIT MORE THAN 1000mg 16 S.B.COLLEGE OF PHARMACY,SIVAKASI

REQUIREMENTS FOR HAIR CREAMS:

REQUIREMENTS FOR HAIR CREAMS S.NO CHARACTERSTICS REQUIREMENT 1 THERMAL STABILITY SSTABILITYSTABILITY TO PASS THE TEST 2 pH 5-9 3 TOTAL FATTY SUBSTANCES CONTENT 15 4 5 TEST FOR RANCIDITY WATER CONTENT,MAX SHALL BE FREE FROM RANCIDITY 85 17 S.B.COLLEGE OF PHARMACY,SIVAKASI

Slide 18:

Test for thermal stability: Spread a 20mm broad &5mm thick stripe from material to be tested on the internal wall of beaker of beaker of 100ml capacity in its total height. Keep beaker for 8 hrs in humidity chamber at 60-70% relative humidity&temperature of 37±1ºC . The cream shall be taken to have passed the test if on removal from the thermostat, no oil separation is observable. 18 S.B.COLLEGE OF PHARMACY,SIVAKASI

Slide 19:

Determination of pH : FOR oil in water type emulsion cream, take 5±0.01g of cream in 100ml beaker. Add 45ml of water & disperse the cream. Determine the pH using Ph METER For w/o emulsion cream -10±0.01g cream +90ml spirit ,warm to 45ºC,stir,filter alcoholic layer,measure.pH of filterate with that meter Test for rancidity: Shake 10ml of material ,melted if necessary,with 10ml conc.hcl and 10ml phlorogiucinol,shake for 1 mts. No pink color indicates that the test passes. 19 S.B.COLLEGE OF PHARMACY,SIVAKASI

Slide 20:

Determination of water: 10g material +200ml toluene +dry pumice stone ,connect apparatus & fill receiving end of trap with toluene poured through of condensor . Heat flask for 15 mts. When toluene begins to boil reflux it to rate of 2 drops per second,until most of water has passed over .then increase rate to about 4 drops per second. When water has apparently all distilled over,rinse the inside of condensor tube with toluene while brushing down the tube brush attached to a copper wire and saturated with toluene.continue distillation for 5mts. 20 S.B.COLLEGE OF PHARMACY,SIVAKASI

Slide 21:

Remove the source of heat ,allow that receiving tube to cool to room temperature.when water &toluene are separated ,read vol. Of water Calculation: Water, %by mass= v-volume of water in ml at room temp collected in receiving tubes. d- density of water at room temperature. M-mass in g of material taken for rest. Vd100/M 21 S.B.COLLEGE OF PHARMACY,SIVAKASI

Slide 22:

Determination of total fatty substance: Total fatty substance=100M1/M2 M1- mass in g of residue M2-mass in g of material taken for rest. Procedure: 2g+25ml dil hcl +refiux until water have separated. Take 300ml into separating funnel,cool to 20ºC Rinse with 50ml ethyl ether in portions of 10ml Separate aqu. Phase &shake it with 50ml ether,until free from acid. Filter the ether extract with fil. Paper contain na .sulphate into conical flask which has been dried at temp60±2ºC Wash sod.sulphate on filter with ether &dry material remaining in flask at temp 60±2ºC to constant mass. 22 S.B.COLLEGE OF PHARMACY,SIVAKASI

SKIN CARE PRODUCTS:

SKIN CARE PRODUCTS Introduction : Cosmetic products which are applied on skin for beautification,protection/other purposes pH 4-5.6(acidic). Available in solids,semisolids,liquids. Solids-powders(body,face) Semi solids-emulsion, creams, lotions. Liquids-monophasic,biphasic S.B.COLLEGE OF PHARMACY,SIVAKASI 23

Slide 24:

S.B.COLLEGE OF PHARMACY,SIVAKASI 24 Pdts marketed under variety of names Cold creams Cleansing creams Cleansing milk Cleansing lotions Vanishing creams emollient creams Skin conditioning creams Moisturing creams Night massage creams. Hand body creams. Sunscreen preparations

Skin powders:

Skin powders Types: Body powders- talcum,toilet,deodorant,dusting Face powders. Ingredients used for face powder : Titanium dioxide,zinc oxide,zn stearate,kaolin(covering) Mg stearate , zn stearate , talc(adhesion) Talc,al hydro silicate( slik soft) Collidal kaolin,starch,bentonite (absorbency) Rice starch,maize (peach like finish) Flowery fragnance /synthetic odour .(perfume) S.B.COLLEGE OF PHARMACY,SIVAKASI 25

Slide 26:

S.B.COLLEGE OF PHARMACY,SIVAKASI 26 INGREDIENTS OF Body powder: Absorbency- kaolin,mg carbonate. Slip- talc,ppt . chalk,starch Adhesion- Kaolin,Zn oxide Antiseptic-Boric Acid,Chloro hemi Acetate

Slide 27:

S.B.COLLEGE OF PHARMACY,SIVAKASI 27 FACE POWDER: Ability to complement skin color by imparting velvet finish to it(smooth finish to facial skin, masking visible imperfection of face and shine due to moisture/grease, from perspiration/screen of skin. BODY POWDER: To absorb moisture/perspiration providing good slip ,cooling effect ,very fine particle size-large surface area resulting in strong light dispersion.

ANALYSIS OF SKIN POWDERS :

ANALYSIS OF SKIN POWDERS Determination of matter insoluble in boiling water: Weigh1 gm of material(wet with little spirit) Add 200ml of water ,boil, allow to settle. Filter(gooch crucible) Wash the residue with water, dry at 105± 2ºC to a constant mass. Matter insoluble in boiling water by %=M1/M*100 Where M1=mass in gm of residue, M=mass in gm of material taken S.B.COLLEGE OF PHARMACY,SIVAKASI 28

Slide 29:

S.B.COLLEGE OF PHARMACY,SIVAKASI 29 DETERMINATION OF FINENESS : 10 gm of material placed in specified sieve 15 Wash with slow stream of running tap water. Dry the sieve containing residue on steam bath Dry the residue to a constant mass at 105± 2ºC Material retained on the specified sieve % by mass= (M1/M)*100 where M1=Mass in gm of the residue retained on specified sieve M=mass in gm of material taken

`:

` Determination of PH of AQ.SUSPENSION: 10g material taken in 150ml beaker Add 90ml freshly boiled and cooled water(stir well) Determine the PH of the suspension using PH meter within 5min TEST FOR LEAD: Preparation of std. lead solution: 1.600g of lead nitrate dissolved in water, make up to 1000ml Pipette out 10ml of solution dilute to 1000ml Pipette out 1 ml of final solution – .01mg of pb S.B.COLLEGE OF PHARMACY,SIVAKASI 30

Slide 31:

S.B.COLLEGE OF PHARMACY,SIVAKASI 31 Procedure: 2g material –incinerate 2hrs (525-550ºC) Cool, add 5 ml perchloric acid takes fumes –hot plate with 3 portions of HF ,cool dil with water filter, Dilute to 200ml,PH(3 to 3.4 ) with dilute ammonium hydroxide yellow to purple color using bromophenol blue indicator,10mg copper sulphate (co – precipitant),ppt sulphides by passing hydrogen sulphide, filter Dissolve the ppt ,with 5ml dilute nitric acid ,wash with hot water and collects washings along with solution in nitric acid .Boil (to remove hydrogen sulphide)

Slide 32:

S.B.COLLEGE OF PHARMACY,SIVAKASI 32 Transfer to nesslers cylinder make ammonical to PH between 8.5 to 10 (Bluish green –to blue with thymol blue indicator Add 5ml of KCN solution ,then add 15ml of hydrogen sulphide solution, dilute to mark and mix Carry out control test using 4ml of standard lead solution and some quantities of reagents as used in test with material. Passed- If intensity of color produced by test with material is not greater than that of produced in control test

Slide 33:

S.B.COLLEGE OF PHARMACY,SIVAKASI 33 Determination of moisture and volatile matter: 5g of material ,dry in hotter oven at temp of 105±2ºc to constant mass Moisture and volatile matter % by mass=(M1/M)*100 TEST FOR ARSENIC: 2g of sample ,incinerate abt 2hrs for at 550ºc Treat with mixture of 5ml con. Sulphuric acid ,5ml con. Nitric acid

Slide 34:

S.B.COLLEGE OF PHARMACY,SIVAKASI 34 Take to fumes on hot plate ,cool and again take to fumes with hydrofluoric acid Cool and dissolve in water up to 100ml From above take 50 ml ,carry out test for arsenic (gutziet apparatus) Using for comparison stain obtained with .002 mg of arsenic oxide.

Requirements for skin powders :

Requirements for skin powders SNO CHARACTERISTICS Requirements for Body powder Face powder 1 2 3. 4 5 6 Matter insoluble in boiling water % by mass Fineness : a)Residue on 75µ is sieve ,% by mass,max b)Residue on 150µ is sieve ,%by mass,max Moisture in volatile matter ,% by mass,max PH of Aq. Suspension Heavy metals ,parts per million ,max Arsenic ,parts per million ,max 90.0 2.0 0.5 2.0 5.5 -10 20 2 90.0 1.0 0.5 3.0 5.5 -10 20 2 S.B.COLLEGE OF PHARMACY,SIVAKASI 35

SKIN CREAMS :

SKIN CREAMS Creams are emulsion type& consistency can vary from a liquid to a separable solid. All skin creams can be classified According to function eg) cleaning,foundation,massage etc., According to characteristics properties eg )cold cream, vanishing creams. According to nature/type of emulsion S.B.COLLEGE OF PHARMACY,SIVAKASI 36

Ingredients used:

Ingredients used Bees wax-borax cold creams Liquefying cleansing creams Vanishing creams Night& massage creams Hand& body creams Mineral oil Isopropyl myristate Acetoglycuride Petroleum jelly Bees wax Borax Preservative Perfume Water. Mineral oil Petrolatum Paraffin wax Bees wax Preservative perfume Stearic acid Potassium hydroxide Glycerin Water Perfume Preservative Mineral oil Petroleum jelly White bees wax Paraffin wax Lanolin Borax Perfume Water Perfume Anti oxidant. Tragacanth Glycerin Titanium oxide Water Perfume Color Preservative. S.B.COLLEGE OF PHARMACY,SIVAKASI 37

Requirements for skin creams:

Requirements for skin creams s.no characterstics requirements 1 2 3 4 Thermal stability Ph Total fatty substance ,%by mass ,max Water content,% by mass, max To pass the test 5-9 15 85 S.B.COLLEGE OF PHARMACY,SIVAKASI 38

ANALYSIS OF SKIN CREAMS:

ANALYSIS OF SKIN CREAMS Microbiological examination of skin creams: 15g pancreatic digest of caesin+5g peptide digest of soybean meal+5g nacl,disslove 1000ml of water. Add 15g of powdered agar, heat until agar is digest, adjust the ph to 7.5 with naoh Distribute in 20ml closed tubes with metal caps& autoclave 20mts at 122ºC After autoclaving store tubes in cool place& use within 3 weeks. S.B.COLLEGE OF PHARMACY,SIVAKASI 39

Slide 40:

S.B.COLLEGE OF PHARMACY,SIVAKASI 40 Procedure : 1g of sample+50ml dilute phosphate buffer(ph 7.2)-conical flask, shake well. Pipette out 1ml portions into 3 sterile petridishes Pour melted& cooled soybean digest agar medium over it& rotate plates to mix.inculate plates at 32ºC for 72ºC for inverted positions. Determine the avg no . Of colonies on soyabean casein digest agar medium plates multiply by 30( diution factor).this will be the m.o/g of sample. If the no. of colonies is recovered from any of plates it can be as less than 50m.o/g. 7

Slide 41:

S.B.COLLEGE OF PHARMACY,SIVAKASI 41 Test for thermal stability: Spread the 20min broad& 5mm thick stripe from material to be tested on the internal wall of beaker of 100ml capacity in its total height. Keep beaker for 8hrs in humidity chamber at 60-70% relative humidity temperature of 37±1ºC Passed- if ,on removal from the thermostat, no of oil separation is observed

Slide 42:

S.B.COLLEGE OF PHARMACY,SIVAKASI 42 Determination of ph: For O/W emulsion type: 5g of cream in 100ml beaker, add 45ml of water, disperse cream in it, determine ph at 27ºC using ph meter. For W/O emulsion type: 10g cream+90ml rectified spirit (ph6.5-7.0).warm to 45ºC,stir-15mts,filter-alcoholic layer through fil . Paper Measure the filterate ph at 27ºC using ph meter.

Slide 43:

S.B.COLLEGE OF PHARMACY,SIVAKASI 43 Determination of total fatty substance content: 2g material+25ml dil. Hcl acid, reflux for to get clear solution, pour 900ml separating funnel, cool to 20ºC Rinse with 50ml ethyl ether in portions of 10ml(conical flask),add rinsing(ether) Shake separating funnel until layer separates. Separate the aqu.phase,shake with 25ml of ether twice. Combine all ether extracts wash them with water, until free of acid(methyl orange) Filter to conical flask with na.sulphate dried at 60±2ºC

Slide 44:

S.B.COLLEGE OF PHARMACY,SIVAKASI 44 Distil off ether ,dry material remaining in flask at temperature of 60±2ºC to constant mass. Total fatty substance mass=(M1/M)*100

Slide 45:

S.B.COLLEGE OF PHARMACY,SIVAKASI 45 Determination of water: 10g material+200ml toluene few pieces of dry pumice stone Connect apparatus fill receiving end of trap with toluene poured through top of condensor . Heat for 15mts,when toluene begins to boil, reflux at rate of 2 drops/sec till most of water has passed over, increase rate to 4 drops/sec When water apparently distilled over, rinse inside of condenser tube with toluene while brushing down tube with tube brush attached to a cu wire &saturated with toluene.

Slide 46:

S.B.COLLEGE OF PHARMACY,SIVAKASI 46 Weigh, wash na.sulphate on filter with ether &combine washings the filterate Continue distillation for 5min then remove source of heat, allow receiving tube to cool to room temperature If any droplets of water are adhering to walls of receiving tube, scrub them down with a brush consisting of rubber band wrapped around a cu wire &wetted with toluene. When water&touene have separated-read the vol. of water. Water% by mass=v*d*100/M V=VOL. OF WATER IN ML(collected by receiving tubes) d =density of water M= MASS IN GM taken at rest 7

References:

References ISI 7123:1993 ANNEX (clauses 4.3,4.4,&4.5) for hair creams ISI 7884:1992 ANNEX(clauses 3.4&table 1)for shampoos. ISI 7679:1978 APPENDIX C (clause 3.2.3) and APPENDIX(clauses 3.3 &6.1 &table 1)for hair creams and oils. 47 S.B.COLLEGE OF PHARMACY,SIVAKASI

Thank you:

Thank you 48 S.B.COLLEGE OF PHARMACY,SIVAKASI

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