Some problems formulation
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This document discusses various problems and solutions related to hair care product formulations and manufacturing. It covers topics like shampoo thickeners and foam stabilizers, conditioners, permanent waving, and more. Some key points include: - Electrolytes, alkalonamides, and polymeric materials are commonly used as shampoo thickeners and foam stabilizers. The amount and type of electrolyte affects viscosity and micelle properties. - Conditioners aim to counteract the negative charge left by anionic shampoo surfactants with cationic surfactants. Conditioning depends on surfactant chain length and charge density. - Permanent waving effectiveness depends on processing time and temperature, reducing agent concentration
Some problems formulation
- 1. 11 Some Problems in Hair CareSome Problems in Hair Care Product Formulations andProduct Formulations and ManufacturingManufacturing Assoc. Prof. Dr. Pleumchitt RojanapanthuAssoc. Prof. Dr. Pleumchitt Rojanapanthu Pharmacy Department, Faculty of PharmacyPharmacy Department, Faculty of Pharmacy Mohidol University, Bangkok, ThailandMohidol University, Bangkok, Thailand
- 2. 22 Shampoos ThickenerShampoos Thickener and Foam Stabilizerand Foam Stabilizer • ElectrolytesElectrolytes • Alkalonamides or the alternativesAlkalonamides or the alternatives • Polymeric materialsPolymeric materials
- 3. 33 • ElectrolyteElectrolyte – ionic density of the solutionionic density of the solution – size and shape of micellesize and shape of micelle • Adding the same cation as that of primary anionicAdding the same cation as that of primary anionic surfactantsurfactant – Eg: amm.chloride amm. lauryl surphateEg: amm.chloride amm. lauryl surphate sod. chloride sod. lauryl ether sulphatesod. chloride sod. lauryl ether sulphate Thickener and Foam StabilizerThickener and Foam Stabilizer
- 4. 44 • Electrolyte should be added as solutionElectrolyte should be added as solution (25% W/W)(25% W/W) • Avoiding local concentration gelationAvoiding local concentration gelation Thickener and Foam StabiliserThickener and Foam Stabiliser
- 5. 55 Viscosity/electrolyte curve for aViscosity/electrolyte curve for a well-formulatedwell-formulated shampooshampoo Preferred viscosity range % electrolyte
- 6. 66 Shampoos which need ThiningShampoos which need Thining • Active matter is highActive matter is high • Contain high levels of electrolytesContain high levels of electrolytes • Large amt. of some amphoterics are presentLarge amt. of some amphoterics are present • Addition of short-chain alcohol or glycol: ethonal,Addition of short-chain alcohol or glycol: ethonal, isopropanolisopropanol – Glycols are preferred (less odor/imflammable)Glycols are preferred (less odor/imflammable)
- 7. 77 AlkalonamidesAlkalonamides • Mono-ethanolamide > effective than di- ethanolamideMono-ethanolamide > effective than di- ethanolamide as foam stabiliser and thickeneras foam stabiliser and thickener • Disadvantage : waxy solidDisadvantage : waxy solid rrequired hot process of mixingequired hot process of mixing • Among the group of lauric, lauric/myristic andAmong the group of lauric, lauric/myristic and coconut mono- and di-ethanolamidecoconut mono- and di-ethanolamide • Lauric mono-isopropanolamide is the most effectiveLauric mono-isopropanolamide is the most effective thickener and foam stabiliserthickener and foam stabiliser
- 8. 88 Alkalonamide alternativesAlkalonamide alternatives • PEG-6000 distearatePEG-6000 distearate • PEG-55 propylene glycol oleatePEG-55 propylene glycol oleate • PEG-120 methyl glucose dioleatePEG-120 methyl glucose dioleate • Effective in systems based on someEffective in systems based on some sulphosuccinates, ethoxylated sorbitansulphosuccinates, ethoxylated sorbitan esters alkane sulphonates, lauryl sulphates,esters alkane sulphonates, lauryl sulphates, low level of free fatty alcohols.low level of free fatty alcohols.
- 9. 99 Polymeric materialsPolymeric materials • Natural gumsNatural gums:: guar, karaya, caragenan,guar, karaya, caragenan, lacus beanlacus bean Find little use in today’s shampoosFind little use in today’s shampoos • Cellulose derivativeCellulose derivative:: hydroxyethyl cellulosehydroxyethyl cellulose (HEC), carboxymethyl cellulose (CMC),(HEC), carboxymethyl cellulose (CMC), hydroxypropyl methycellulose (HPMC)hydroxypropyl methycellulose (HPMC)
- 10. 1010 PerfumesPerfumes • Simply added after any hot process is completeSimply added after any hot process is complete • Solubilty problem:Solubilty problem: – Premixing with a suitable solubiliserPremixing with a suitable solubiliser – Ratio of mixing being determined by trial andRatio of mixing being determined by trial and errorerror • PEG-40 hydrogenated castor oil is mostly usedPEG-40 hydrogenated castor oil is mostly used • Polysorbates may cause thiningPolysorbates may cause thining – Premixing with alkalonamide at < 40 CPremixing with alkalonamide at < 40 C
- 11. 1111 PreservativesPreservatives • Most surfactants are already preservedMost surfactants are already preserved • Chosen preservative system should pass aChosen preservative system should pass a recognised challenge test in the finalrecognised challenge test in the final formulationformulation – Freshly preparedFreshly prepared – AgingAging – Accompanied by meaningful preservativesAccompanied by meaningful preservatives assaysassays
- 12. 1212 Opacifier and PearlisersOpacifier and Pearlisers • Aesthetic reasonAesthetic reason • Occasionally used technique for unclear productOccasionally used technique for unclear product Suggestion methodSuggestion method • Buying ready made pearlised base (cheap)Buying ready made pearlised base (cheap) – Make dilution adding to shampoo as hot mixingMake dilution adding to shampoo as hot mixing • Buying highly concentrated pearlising agent (moreBuying highly concentrated pearlising agent (more expensive)expensive) – Adding as cold mix (2%)Adding as cold mix (2%)
- 13. 1313 Conditioning agentsConditioning agents • Back-bone surfactants in shampoos mostlyBack-bone surfactants in shampoos mostly are anionic surfactantsare anionic surfactants • Majority active conditioning agents areMajority active conditioning agents are cationic surfactantscationic surfactants
- 14. 1414 Problem solvingProblem solving • Including more % of amphotericIncluding more % of amphoteric surfactantssurfactants • Reducing charge of anionic and cationicReducing charge of anionic and cationic surfactants by ethoxylationsurfactants by ethoxylation • Replacing cationic surfactants by usingReplacing cationic surfactants by using cationic polymercationic polymer • Adding high level of nonionic surfactantAdding high level of nonionic surfactant
- 15. 1515 Colour fadingColour fading • Stability to pH variation and light can beStability to pH variation and light can be predictedpredicted • Interaction between colour and theInteraction between colour and the complexation of modern shampoo basecomplexation of modern shampoo base evaluated for each formulationevaluated for each formulation – Natural sunlight (shelf life)Natural sunlight (shelf life) – Accelerated conditionsAccelerated conditions
- 16. 1616 Colour fading (con.)Colour fading (con.) • Minimised colour fading by incorporationMinimised colour fading by incorporation of suitable UV absorberof suitable UV absorber • Benzophenone – 4 and –2 water solubleBenzophenone – 4 and –2 water soluble absorbers are most popular (0.05 – 0.1%)absorbers are most popular (0.05 – 0.1%) • Colour should be added as a solutionColour should be added as a solution
- 17. 1717 ConditionersConditioners • Hair charge surface negativeHair charge surface negative • Anionic surfactants for shampooAnionic surfactants for shampoo (usually C(usually C1212 /C/C1414) negative charge) negative charge • Cationic surfactants for conditionerCationic surfactants for conditioner (usually C(usually C1616 / C/ C1818 and quart with Cand quart with C2222)) positive chargepositive charge
- 18. 1818 Conditioners (con.)Conditioners (con.) • Some quarts are relatively poorlySome quarts are relatively poorly biodegradablebiodegradable • ‘‘Ester quarts’is claimed to be betterEster quarts’is claimed to be better • Properties related to charge densityProperties related to charge density • Highly charged cation more stronglyHighly charged cation more strongly attached to the negative-charged hairattached to the negative-charged hair surfacesurface
- 19. 1919 Conditioners (con.)Conditioners (con.) • On the hair surface:On the hair surface: – number., shape and size of fatty acid chain innumber., shape and size of fatty acid chain in molecule are the determinantmolecule are the determinant • A quart with two fatty acid chains providesA quart with two fatty acid chains provides more lubricity than a quart with onemore lubricity than a quart with one • More longer chainMore longer chain >>effective lubricanteffective lubricant than shorter onethan shorter one
- 20. 2020 Conditioners (con.)Conditioners (con.) • Using single fatty acid chain greasy hairUsing single fatty acid chain greasy hair / frequent use/ frequent use • Using twin fatty acid chain on theUsing twin fatty acid chain on the dried / damaged hairdried / damaged hair
- 21. 2121 ManufacturingManufacturing • Simply diluting down a suitable quart with waterSimply diluting down a suitable quart with water • The stability and effectiveness maybe limitedThe stability and effectiveness maybe limited • The appearance of emulsion may be course andThe appearance of emulsion may be course and grainy in texturegrainy in texture • Low opacity/ the flow has high yield pointLow opacity/ the flow has high yield point • Increased viscosity with timeIncreased viscosity with time • Sensitivity to change manufacturing methodSensitivity to change manufacturing method
- 22. 2222 Problem solvingProblem solving • Introduction of other waxy component: estersIntroduction of other waxy component: esters – Decrease H-bonding with OHDecrease H-bonding with OH-- __of fatty alcoholof fatty alcohol – Decrease the viscosity risingDecrease the viscosity rising • Addition of small amount of oilAddition of small amount of oil – Smooth out the emulsionSmooth out the emulsion – Increase opacityIncrease opacity – Facilitate processingFacilitate processing – Easier to obtain repeatable viscosityEasier to obtain repeatable viscosity
- 23. 2323 Problem solving (con.)Problem solving (con.) • Additon of a non-ionic to the emulsionAdditon of a non-ionic to the emulsion – Can increase grealty in the emulsificationCan increase grealty in the emulsification – Increase stability due to the formation of mixedIncrease stability due to the formation of mixed micelles and the presence of mixed surfactantsmicelles and the presence of mixed surfactants at the oil/water interface of the emulsionat the oil/water interface of the emulsion
- 24. 2424 Bodying AgentsBodying Agents • As shampoos, conditioners perceived to beAs shampoos, conditioners perceived to be more effective when thick and creamymore effective when thick and creamy • Using high levels of fatty alcohols withUsing high levels of fatty alcohols with other waxy estersother waxy esters – Improvement in handling of hair especiallyImprovement in handling of hair especially when combingwhen combing
- 25. 2525 Auxilliary EmulsifiersAuxilliary Emulsifiers • Depending on HLBDepending on HLB • Some quart mols. have emulsifierSome quart mols. have emulsifier properties, some are notproperties, some are not • Incompatibilty with anionic emulsifiersIncompatibilty with anionic emulsifiers • Addition of non-ionic are preferredAddition of non-ionic are preferred • Recommended to use two emulsifiers (highRecommended to use two emulsifiers (high and low HLB)and low HLB)
- 26. 2626 ThickenersThickeners • Cationic emulsion do not usually requiredCationic emulsion do not usually required thickenerthickener • If needed, they usually response to salt in aIf needed, they usually response to salt in a similar way as shampoosimilar way as shampoo • The method of using thickening must beThe method of using thickening must be treated with extreme cautiontreated with extreme caution • Irreversible emulsion breakdown should beIrreversible emulsion breakdown should be avoidedavoided
- 27. 2727 SuggestionsSuggestions • Add only small amount of salt solutionAdd only small amount of salt solution at a time since viscosity will peak atat a time since viscosity will peak at much lower salt level than that ofmuch lower salt level than that of shampooshampoo • Add salt solution at cold emulsionAdd salt solution at cold emulsion (max 30 C)(max 30 C) • Shear rate has effect on the emulsion;Shear rate has effect on the emulsion; moderate shear rate should be usedmoderate shear rate should be used • Try small scale before scaling upTry small scale before scaling up
- 28. 2828 • Gum-type thickener: cellulose derivativeGum-type thickener: cellulose derivative dominate for clear conditionerdominate for clear conditioner • Carbomers incompatibility withCarbomers incompatibility with cationicscationics Suggestions (con.)Suggestions (con.)
- 29. 2929 Permanent WavingPermanent Waving Factor affecting the efficiency of the productsFactor affecting the efficiency of the products • Processing timeProcessing time • Processing temperatureProcessing temperature • Concentration of reducing agentConcentration of reducing agent • Ratio of lotion to hair quantitiesRatio of lotion to hair quantities • Penetration of the lotionPenetration of the lotion • pHpH • The nature and condition of untreatedThe nature and condition of untreated hairhair
- 30. 3030 • Procession timeProcession time – Should not be longer than necessaryShould not be longer than necessary – Home perm may be designed for longer processingHome perm may be designed for longer processing • Processing temperatureProcessing temperature – Will be ambient for most productsWill be ambient for most products – For hot process: needs external mean of heat orFor hot process: needs external mean of heat or exothermic chem. reaction (mixing before use)exothermic chem. reaction (mixing before use) Permanent Waving (con.)Permanent Waving (con.) Factor affecting the efficiency of the productsFactor affecting the efficiency of the products
- 31. 3131 • Concentration of active ingredientsConcentration of active ingredients – A wide range of concentration is availableA wide range of concentration is available – Will not be changed during use except by dilutionWill not be changed during use except by dilution • The ratio of lotion to hairThe ratio of lotion to hair – Insufficient lotion to treat when very long hair isInsufficient lotion to treat when very long hair is involvedinvolved Permanent Waving (con.)Permanent Waving (con.) Factor affecting the efficiency of the productsFactor affecting the efficiency of the products
- 32. 3232 • The penetration of the lotionThe penetration of the lotion – Enhanced by the inclusion of surfactantEnhanced by the inclusion of surfactant – Mostly non-ionic and anionicMostly non-ionic and anionic – Hydrogen bond breaker: ureaHydrogen bond breaker: urea Permanent Waving (con.)Permanent Waving (con.) Factor affecting the efficiency of the productsFactor affecting the efficiency of the products
- 33. 3333 • pHpH – Too low product doesn’t work wellToo low product doesn’t work well – Too high severe hair damageToo high severe hair damage andand high irritationhigh irritation of the skin of scalpof the skin of scalp – Maximum bond cleavage occurs at pH 9Maximum bond cleavage occurs at pH 9 > 8.5 bond reformation is less complete> 8.5 bond reformation is less complete < 7.5 amt. of bond cleavage is low and< 7.5 amt. of bond cleavage is low and reformation is more completereformation is more complete Permanent Waving (con.)Permanent Waving (con.) Factor affecting the efficiency of the productsFactor affecting the efficiency of the products
- 34. 3434 - Conventional ammonium thio-glycollate lotion- Conventional ammonium thio-glycollate lotion Approx 9.2Approx 9.2++ 0.20.2 - pH is currently restricted by law to a max 9.5- pH is currently restricted by law to a max 9.5 and total thio-glycollate to 8% (free acid)and total thio-glycollate to 8% (free acid) Permanent Waving (con.)Permanent Waving (con.) Factor affecting the efficiency of the productsFactor affecting the efficiency of the products
- 35. 3535 • Hair type and conditionHair type and condition – Coarse hair require more severe treatmentCoarse hair require more severe treatment – Fine and damaged hair require gentleFine and damaged hair require gentle treatmenttreatment Permanent Waving (con.)Permanent Waving (con.) Factor affecting the efficiency of the productsFactor affecting the efficiency of the products
- 36. 3636 • Other Variables:Other Variables: – Number and diameter of the rollerNumber and diameter of the roller – Tension of the hair on the rollerTension of the hair on the roller – The speed at which the operation is carried outThe speed at which the operation is carried out Permanent Waving (con.)Permanent Waving (con.) Factor affecting the efficiency of the productsFactor affecting the efficiency of the products
- 37. 3737 Product Evaluation and TestingProduct Evaluation and Testing Methods of testing and evaluating productsMethods of testing and evaluating products are essential to confirm that products areare essential to confirm that products are met the requirementsmet the requirements • In vitro method: lab-based instrumentalIn vitro method: lab-based instrumental techniques for initial screeningtechniques for initial screening • In vivo method: salon or consumer testingsIn vivo method: salon or consumer testings
- 38. 3838 • EC “Cosmetic Directives specify that : “ProductsEC “Cosmetic Directives specify that : “Products should remain safe and effective for two andshould remain safe and effective for two and a half years”a half years” The Test Methods:The Test Methods: – High and low temperature storageHigh and low temperature storage – Freeze / thawing cyclingFreeze / thawing cycling – CentrifugationCentrifugation – etcetc Stability TestingStability Testing
- 39. 3939 Compatibility TestingCompatibility Testing • The compatibility testing should be carried outThe compatibility testing should be carried out • Two sets of tests to be runned in parallelTwo sets of tests to be runned in parallel – One set in actual containers to be usedOne set in actual containers to be used – The other in inert container, usually glassThe other in inert container, usually glass • Should give valuable comparative dataShould give valuable comparative data
- 40. 4040 Claim JustificationClaim Justification • If there is specific claim, the manufacturerIf there is specific claim, the manufacturer mustmust be able to justify:be able to justify: – Known properties of raw materialsKnown properties of raw materials – Usage level and condition of useUsage level and condition of use – Lab testing, salon trialsLab testing, salon trials • consumer panel test: the no. and type of subjectsconsumer panel test: the no. and type of subjects
- 41. 4141 Product SafetyProduct Safety • If a formulation is a ‘standard’ one, no furtherIf a formulation is a ‘standard’ one, no further action is necessaryaction is necessary • If new raw material/unusual combinations ofIf new raw material/unusual combinations of materials are usedmaterials are used • If any ingredient is present at an unusually highIf any ingredient is present at an unusually high levellevel
- 42. 4242 Product Safety (con.)Product Safety (con.) • The opinion of a qualified dermatologist,The opinion of a qualified dermatologist, ophthalmologist, toxicologist may be an valuableophthalmologist, toxicologist may be an valuable backup to the cosmetic chemist’s judgementbackup to the cosmetic chemist’s judgement • If there is real doubt about the total safety,If there is real doubt about the total safety, further testing should be in the form of humanfurther testing should be in the form of human volunteer studyvolunteer study
- 43. 4343