Home Cosmetic Science Talk Formulating Stability problem with anhydrous balm

  • Stability problem with anhydrous balm

    Posted by MariaSibon on February 20, 2023 at 4:37 am

    Dear All,

    I am designing a foot balm and I am puzzled since everytime I think I found the perfect blend, an esthetic instability occurs. The problem is identified in the BASE blend and I have ruled out the essential oils and actives effect. It must be a fat component crystalisation issue that occurs in T>5, T<40 C . I observe it in my bench sample at T=18C. Little crystals like spots appear in the balm which when spread on skin they are melting. The strange thing is that my sample at 40C, and 5 C is very good consistency, no grainy effect at all. I have read several articles mentioning that high stearic acid fats such as shea butter, mango butter, cocoa butter can cause this grainy effect. Some recommendations are extending the heating time when melting the fats and rapid coolling after molding.

    Unfortunately rapid cooling complicates things during production and it is not an option right now, do I have any other alternatives? Any recommendations? Please find a picture that the grainy effect appears like small spots. Thank you in advance

    Let me give you a little more details about the ingredients:

    1. Beeswax 13,0%

    2. Mango butter 12,0%

    3. Isopropyl Myristate 12,0%

    4. Cetearyl Alcohol 12,0%

    5. Coconut oil 11,0%

    6. Castor oil 10,0%

    7. Cocoa butter 10,0%

    8. Polysorbate 20 6,0%

    9. Almond oil 4,5%

    10. Rosehip oil 4,5%

    11. Actives and Essential oils up to 100%

    MariaSibon replied 1 month ago 3 Members · 9 Replies
  • 9 Replies
  • graillotion

    Member
    February 20, 2023 at 2:41 pm

    If it is simply….butters recrystalizing….then search ChemicalMatt’s comments on this topic….as he has answered it half a dozen times…. (Maybe search under polyglyceryl’s.)

    • MariaSibon

      Member
      February 21, 2023 at 2:57 am

      @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!

      • graillotion

        Member
        February 21, 2023 at 3:03 am

        No problem….I actually read all 44 pages of Matt’s comments last week (good thing it was raining like crazy ….no yard work)….while searching on another topic. He is a valuable asset to the community!

        I could have tossed you the answer….but there is SO MUCH value….in discovering it yourself…and all the learning that came along with it. 🙂 Good Luck.

        • This reply was modified 9 months, 1 week ago by  Graillotion.
        • MariaSibon

          Member
          February 21, 2023 at 4:07 am

          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 9 months, 1 week ago by  MariaSibon.
  • MariaSibon

    Member
    October 26, 2023 at 8:00 am

    @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!

  • chemicalmatt

    Member
    October 26, 2023 at 12:41 pm

    Two insights to share here @MariaSibon . The polyglyceride ester is competing with polysorbate 20 here, so reduce the polysorbate 20 to 1.0% and increase the PG-3 diisostearate up to 2.0 - 3.0% and see what happens (not sure what polysorbate-20 is doing there in first place but I’ll leave that to you.) The other is that cocoa butter and coconut oil is the sole crystallization problem here, mango butter is actually composed chiefly of hydrogenated vegetable oil which is more stable. The only other aspect - a stretch here - is that the 6.0% or more of essential oils is “solvent stripping” beeswax of its unsaturated fatty acids which are then precipitating. That’s all I got.

    • MariaSibon

      Member
      October 27, 2023 at 3:38 am

      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.

  • graillotion

    Member
    October 26, 2023 at 2:43 pm

    I can only bask in the glow of Matt’s intellect. But I can often times see the elephant in the room. 😄 🐘

    Follow Matt’s advice, but consider this….can you sub the butter with Murumuru? It is almost devoid to stearic acid…which is in a nutshell….the issue. 🙂

    Give it a try.

    • MariaSibon

      Member
      October 27, 2023 at 4:04 am

      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.

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