[MariaSibon]

Dear PeiHoong,

I understand this is an old post, but I would be interested to know if you have realised what is causing your unstability and how you have solved it.

I presume it is your low-melting butters in your fomulation partially melting and recrystalising creatiung the white spots.

I have a similar problem with an anhydrous balm formlation that after a few months fat blooming occurs and I am working on reformulation and process improvement to minimise the risk of fat blooming as I cannot get rid of the balms.

I would be grateful if you could share any feedback experience you might have.

[MariaSibon]

@Graillotion @chemicalmatt

Hello all and specifically graillotion and chemicalmatt, I hope it is not a problem tagging you, but I understand you have a lot of experience in this matter and I would appreciate your input.

So I went though this “Ithaka journey” and I thought I reached a final destination but unfortunately the journey is still on.

Meaning I went through a anhydrous balm formulation for a foot balm marketed to include natural emollients and aroma. We reached to a formulation mentioned before that after a few months stored in RT we discovered the fatty acids re-crystalisation issue that commonly this balms have, especially when including shea, mango, cocoa butter etc.

After many suggestions and specifically inputs by grailotion and chemical matt which I am very thank ful for, I concluded to incorporate a polyglyceryl emulsifier trying to prevent recrystalisation issue.

I concluded to the below formula:

beeswax13%

isopropyl myristate herbal extract 12%

mango butter 12%

cetearyl alcohol 12%

coconut oil 10%

cocoa butter 10%

castor oil 10%

polysorbate 20 5%

almond oil 4,5%

rosegip oil 4,5%

polyglyceryl-3-diisostearate 1%

salicylic acid 1%

tocopherol, 0,5%

tocopheryl acetate 1%

essential oils blend 2%

Lab sample at RT (20-30C) is OK until 23 weeks(now) but production scale up to 7 kg of the same formulation did the bloom. presumably from 1 week, noticed at 8 weeks.

Optimising formula to 4%polyglyceryl-3-diisostearate and decreasing 3% of mango/cocoa butter, same production scale and process, we noticed the bloom at 1 week.

I give pictures below respectively.

Customer wants to launch as soon as possible, but how am i going to test the blooming without waiting for long enough? is thee an “accelerated prediction”?

I know that if I replace the butters causing it it will be an ease of mind, but this is not an option, I have to keep the ingredients and tailor accordingly.

What is the optimum low concentration for mango/cocoa butter to prevent blooming?

All Samples were not rapidly cooled after production. Will cooling prevent the blooming efficiently?

I am afraid the target market is hot climate and there will be critical temperatures for fat liquification and polymorphism (20-40C).

I would appreciate your valuable input!

[MariaSibon]

This is from EU ANNEX III, restrictions.

no salicylic acid is allowed for kids below 3 years old.

My question is for (b) category…It is allowed up to 2% in a face product but not a body lotion?

I am developing a foot balm with salicylic acid. Is it in b or c category? it is for foot use not body.

I would prefer to use 1% instead of 0.5% and I am not sure what to do.

[MariaSibon]

Hello,

I would like to share my humble experience in this topic.

We are trying to finalise formulation of a foot repairing balm which is anhydrous.

Among the ingredients I use salicylic acid 0.5% which is listed also as preservative in cosmetics, and 2% overall essential oils which literature suggests they have antimicrobial effect.

Micro test of sample 40C, 6 weeks failed on total count bacteria (6000, when limit is 1000).

I cannot measure the water content, but after looking the specifications of my ingredients in more detail, I might have 3-5% moisture. Also chatting with my safety assesor, many besswax ointments that are consider anhydrous and safe fail micro test, it may have to do with beeswax and the tendency to bind water.

We have decided to include preservative in our formula. This looks unfair (from a marketing point of view) to similar products in the market that claim “preservative free” and therefore more “natural”, but we know that we are on the safe side.

Checking the presence of e.g. phenoxyethanol to various anhydrous productw in the market, you will find plenty.

So please consider this to your lipstick formulation, selection of ingredients and preservatives.

[MariaSibon]

Is there a specific reason that you blend the isopropyl myristate at the end?

[MariaSibon]

I do not see any picture to see the colour.

But bare in mind that if it is an old sample decoloration might occur due to the fragrance decomposition to colorful substances such as vanillin. If it a “sweet” fragrance it is very likely to contain high content of vanillin.

[MariaSibon]

As far as I understand, TEC inhibits the breakdown of sweat to malodorous substances, while deoplex does not inhibit the breakdown but neutralises the malodourous substances by converting them in salt that does not smell.

I do not know which one is more efficient, but I would prefer TEC mechanism, to prevent the production of smelly substances in the first place.

[MariaSibon]

What is your other variations you are comparing to? if i understand well, I am assuming separation happens on top, because of inefficient emulsification. if your are trying to make a “gel type” wax based on water&ceteareth-25, beeswax is not needed. At least not for thickening.

What is your benchmark?

[MariaSibon]

@Lab
Perhaps if you are using already a significant amount of PEG-40 Hyd. Castor oil, you did not observe any benefit of glycerin during processing with your waxes? Bare in mind that this might not be so easy to see in lab scale but it might create problems when scaling-up.

I am already using 30% Cet-25 for an aqua based pomade and I am trying to make a new product with similar ingredients but even harder. I played with the “plasticisers” ratios but I ended up that it only becomes harder if I increase cet-25, for example up to 33% makes a significant difference. 
However, that increases the set point, it solidifies very quickly, around 70C and makes processing hard.

I am wondering if I increase more the “plasticisers” like Propylene Glycol, Peg-40 Hyd. Castor oil, polysorbate 20, Peg-7 Glyceryl Cocoate and keep 33% cet-25, will lower the set point, but still leave a hard texture on the final gel wax?

Any thoughts?

[MariaSibon]

Hello,

Thank you for your comments.

@Bill_Toge. I am generally avoiding to use the PVP types as they are prone to flaking and leave residues on hair, as you already mentioned. I also have not seens it aomng ingredients lists in other benchmarks.

The mystery must be around some new polymer fixatives, I have seen listed polymers such as
polyacrylate-2 crosspolymer
acrylates copolymer

But these could imply hundreds of products I guess.

I tried polyacrylates-2 crosspolymer (Fixate superhold), but did not like the effect at all.

[MariaSibon]

Thank you all for your suggestions, I will review.

[MariaSibon]

Thank you for your reply.

Oh the elephant is big! I forgot to upload the nasty picture of 2 months production sample.

See below.

I wish I could predict the crystalisation issues beforehand and use alternative butters.

The customers request is know to use the same materials as there cannot be used somewhere else, so I ideally i have to tailor ratios and fix the problem or solve this process-wise.

I have read many people using rapid cooling to solve this, I see professional balm machines incorporating cooling method after filling. I wonder if this is the only way.

[MariaSibon]

Dear chemicalmatt, thank for your quick respond and valuable advise.

1) I have incorporated cetearyl alcohol and polysorbate 20 in order to dissolve salicylic acid in the initial oil blend without PG-3 diisostearate. I did reduced the amount of polysorbate 20 when added PG-3diisostearate, but never tried to remove or dramatically reduce it, not sure if salicylic acid will be still dissolved in this case. also I have a trial with more 6% polysorbate 20/1% PG-3 that showed a much better fat bloom profile (5 months so far no bloom) while the 5% polysorbate 20/1%PG-3 appeared bloom in the 4+, although increases in critical butters might have caused that.

I am trying to understand what is the mechanism of PG-3 in the blend , I understand that somehow creates a crystal latex that promotes V stable polymorph of cocoa butter and prevents oils leaking/separation. Do you have any article to suggest to further study this?

Is this mechanism protecting the balm from temperature fluctuations? Consumes will use it in high climates 25-35 C.

2)What is the problem with coconut oil and cocoa butter? I have seen it in many cosmetic balms. How do they do it I wonder? 🙂 Are they imcombatible? Is lauric acid triglycerols promote unstable polymorphs of cocoa/mango butter?

How can I fix this?

3) My mango butter fatty acids profile is very close to cocoa butter .

mango major fats: Stearic 45%, Oleic 36% Palmitic:13%,

cocoa butter : Stearic 37%, Oleic 32% Palmitic: 26%

So I presume mango and cocoa contributes similarly to the fat recrystalisation problem.

4)Thank you this is useful , I presume it is not my critical factor here, where my problems is more with the mango/cocoa butter that are critical for fat re-crystalisation.

I have noticed my cocoa raw material has shown blooming on the surface of pellets.

I know I have to make sure during the process that teh fats are well melted and the mixture is clear, but is there any chance nucleous of unstable polymorphs to survive and initiate the bloom?

there is a though to melt and rapid cool cocoa butter before production to vanish existing blooming. Do you think this will help?

5)Do you have experience with rapid cooling?

I am wondering if the rapid colling mechanism (temperature control of polymorphs kinetics) in conjuction with the PG-3 mechansim will make a product more stable to temprature fluctuations

6) Finally how to I test/evaluate my trials in short time? Do I have to wait 6 months and more or is tehre an accelerated method to stess the bloom and predict its behaviour in shorter time?

I know I ask a lot, but I am so full of questions marks!?!?!?!?!

Hoping to a fruitful discussion here, Thank you in advance.

[MariaSibon]

Hello,

I presumed so far you have solved the problem…Any updates?

My small experience says that you need some lipids in you formula to act as plasticisers that is why most of basic formulation for aqua waxes based on high concentrations of ceteraeth-25/30 uses ingredienst such as PEG-40 Hydrogented castor oil, polysorbate 20, peg-7 glyceryl cocoate or some emollients which help with smooth physical transitions during processing but also I presume it will help with flaking.

[MariaSibon]

Yes, my understanding is that wart removers is under pharmaceuticals regulation.

Any dermaceutical, cosmeceutical or cosmetic with medical claim, still need to comply with cosmetics regulation…It is really a grey area….

Regarding salicylic acid safety assessment @fareloz made a really good comment that did not think initially. See here: https://chemistscorner.com/cosmeticsciencetalk/discussion/salicylic-acid-and-the-kiddos/#

The factor of surface area plays a great role during toxicological assessment. e.g. face serum is allowed to have 2% but body lotion only 0.5%, because of the larger area of application and therefore absorption. Maybe the same goes for warts because it is applied only in a small spot?

Salicylic acid and the kiddos…….

[MariaSibon]

Thank you very much for your insightfull comment! ok, that makes sense f you include the surface area factor in the safety assesment.

I still believe it is rather unclear, but I agree, a foot balm has a clear application, feet, heels not body so it should be category b.

Thank you!

[MariaSibon]

Thank you for your comment.

Yes, I am aware for the pH effect on hair, although I believe for a styling product a pH 5-5,5 is good enough.

I understand that if I am using the Sodium Benzoate and Potassium Sorbate blend I will need to optimise the pH to 4,5-5 as you suggest as this will optimise the preservation efficiency, although supplier claims it works up to pH 5,5.

Is the powder easily dissolved in water phase? Any compabitibility issues that I should be aware?

Thank you

[MariaSibon]

Thank you for your comment.

Yes that is right, my formulation variations are in the range of pH =5,0-5,5, so using on a blend of Sodium Benzoate and Potassium Sorbate salts it would not be a problem. I am not interested for “natural” or “eco” claims, I just want to make sure preservation system will be efficient, as I have seen many cases of matte waxes go bad in the market, or have very short PAO.

[MariaSibon]

Thank you very much for your comment.

So, if I understand well, you think 1,3 is more marketing than suitable preservatives?

With regards to organic acids, my supplier has the option of ready to use :

i)Phenoxyethanol+Sorbic Acid, Benzoic acid

and another option of powder blend of

ii) Sodium Benzoate and Potassium Sorbate.

If I understand well your comment, even if I manage to solubilise (i) in my preparation, will their efficiency be limited due to low solubility of organic acids in the water phase?

Do you think (ii) will more efficient versus (i)?

I apologise in advance for my multiple questions, I am trying to learn more regarding preservatives since it is difficult to source information from suppliers regarding their efficiency and suitability in products.

[MariaSibon]

I leave this:

“As you set out for Ithaka

hope the voyage is a long one,

full of adventure, full of discovery….

…And if you find her poor, Ithaka won’t have fooled you.

Wise as you will have become, so full of experience,

you will have understood by then what these Ithakas mean”. Constantine Cavafy

• This reply was modified 1 year, 2 months ago by  MariaSibon.

[MariaSibon]

@Graillotion Thank you, indeed there are several discusions on this topic, I have learnt a lot.

I am ordering some polyglyceryl fat esters of low HLB for further trials.

Many thanks!

[MariaSibon]

@kajalthakur

Hello, I am also facing the same problem for my anhydrous foot balm formulation. I use around 20% of fats high in stearic acid (cocoa butter, mango butter). I have researched and I found some suggested practices.

1)making sure sufficient heating is done, such as mixing fats at 80C, 20 min.

2) Apply rapid cooling after molding

3) Use polyglyceryl fat esters to avoid crystalisation as very wisely @chemicalmatt and others mentioned several times.

I havent tested the above thoroughly, however I do apply step 1 in every lab batch I produce.

I did notice that my 5C, 40 C sample did not make any recrystalisation, but the 18-20C sample did.

So I am working on confirming if rapid cooling will solve our problem for manufacturing or I need to add polyglyceryl fat ester to be on the safe side.

Could you share your experience? Did you manage to solve the problem by only optimising the manufacturing process using steps 1 and 2?

Thank you in advance

[MariaSibon]

Hello, do you think another low HLB emulsifier like SPAn 80 could be used to avoid crystalisation of high stearic acid butters? I have some problems in my formulation for a foot balm. The product it is ok at 5C, ok at 40C but at 20 C, small crystals are created uniformly inn the balm, that gives that grainy feel when spreading. i am preparing a post about this with all info, I just saw your comment here and found it very helpful

[MariaSibon]

Well done!

We are also working on a matte aqua based wax where the key ingredient is again ceterareth-25, combining with hard fat waxes (beeswax, hydrogenated vegetable waxes, cetearyl alcohol etc), kaolin to make a thick milky matte emulsion. I have obtained several good bases but need to increase structure/thickness and I wondering with with ingredients I should experiment more. Is it again cetereth-25 the game-changer or do I need to invest on hard fat waxes? For example I saw an improvement when replacing beeswax with hydrogenated castor oil.

Any insights?

[MariaSibon]

Did the supplier notify you that you need to mix the product before using?

This is serious if separation happened. I am also waiting for a sample of keratin product from Active Concepts for a new project, and now I worry that the products might not be reliable.

The one I am going to use is oil soluble aminoacids derived from plants, with apricot kernel oil as a base, no silicones: “AC Vegan Keratin OS” (Prunus Armeniaca (Apricot) Kernel Oil Lens Esculenta (Lentil) Seed Extract & Hydrolyzed Cicer Seed Extract & Chenopodium Quinoa Seed Extract).

I want to blend it on a plant oils mixture for a nail conditioning product.

Hope it works, I can update you if interested.