Stabilize Vitamin C

mflick1mflick1 Member
edited December 2013 in Formulating
Hello,

I'm trying to stabilize Vitamin C in a serum, I've already made which seems like ten failed bench samples... Any suggestions??? 

Thanks
Mindy

Comments

  • BobzchemistBobzchemist Member, PCF student
    Keep it away from oxygen  and water...
    Robert Zonis, Sr. Formulation Chemist, Beaumont Products "All opinions and comments expressed are my own, have no relation to Beaumont Products, are fully copyrighted, and may not be used without written permission."
  • PerryPerry Administrator, Professional Chemist
    This isn't an easy problem to solve.  Like Robert says, make an anhydrous formula.
    Learn to formulate cosmetics
  • mflick1mflick1 Member
    Yes, I've been trying for awhile to do this and have had no success thus far. My formula now consist of no water and it only last about 7-10 days before it starts to turn really yellow. Is there any chemicals that have been shown to help stabilize Vit C at all? How do the big companies get a 20% stabilized Vit C serum but so many people can't figure it out? Or is the question maybe that it's not being stabilized but consumers really don't know the difference anyway? I've seen my share of bad, terrible and plan shouldn't be on the shelf cosmetics. 

    Also, would a nitrogen puff before induction sealing help keep shelf life of my Vit C formula? 
  • pmapma Member
    L'oréal (Skinceuticals) stabilizes vitamin C with ferulic acid and vitamin E. But theirs serums still oxidize easily. You buy them with a champagne color and after some days they are brownish. 

    What about using vitamin C derivatives, like magnesium ascorbyl phosphate? 
  • PerryPerry Administrator, Professional Chemist
    I think it the reality is that consumers can't tell a difference whether their vitamin C is oxidized or not.  All that matters to people is that they are putting something on their skin that says Vitamin C.  The things that make the formula actually work (moisturizers, occlusive agents, etc) are what's responsible for whether people like a product or not.

    For the most part, unless you're getting a prescription dose of Retinol, vitamins in cosmetic products have no effect on the results.  At least I haven't seen any real-life evidence that they do.
    Learn to formulate cosmetics
  • simonasimona Member
    why not use ascorbyl tetraisopalmitate instead?
  • pmapma Member
    I agree with Perry, but the the combination of ascorbic acid (vitamin C) + ferulic acid + tocopherol in the right pH can help protect your skin from the sun:






    Vitamin C also has an anti-melanogenic effect, so can help to diminish spots... 
  • PerryPerry Administrator, Professional Chemist
    @pma - Interesting studies.  They were pretty small though <20 subjects in them all and they didn't provide an adequate control in my view.  

    They did what many people do when investigating cosmetic products / ingredients.  They missed the most important control.

    In these studies, the question isn't whether Vitamin C can protect skin from the sun, the question is can Vitamin C protect skin from the sun better than the best technologies (e.g. traditional sunscreens).  Since they didn't include them, I'm guessing the answer is 'no'.  

    Therefore, for a formulator the best strategy would be to create a sunscreen using traditional sunscreens and add a drop of Vitamin C to make the claim that it is in there.
    Learn to formulate cosmetics
  • mflick1mflick1 Member
    I looked down that path but derivatives but get mixed results in how effective they are compared to L-ascorbic acid. Well I guess if I figure it out, I'll be keeping my process ultra secret!
  • MicroformulationMicroformulation Member, Professional Chemist
    I believe that the use of Vitamin C with Ferrulic acid is protected under patent.

    I have had good luck with an anhydrous formulation based upon silicones. The ascorbic acid is soluble in PEG-8. The background for the Formulation is outlined in a C&T Article from 2006.

     https://drive.google.com/file/d/0BwuqL_fQzYhiZjB5SFFDZ2JaU3c/edit?usp=sharing
    markfuller@microformulation.com Microformulation.com Microformulation Cosmetic Consulting provides Custom Formulations for both large Commercial accounts as well as smaller entrepreneurs. We can provide Naturally compliant Formulations under the NSF, NPA, Whole Foods and USDA Organic Certifications. BS.Pharm Albany College of Pharmacy, Union University.
  • RubenRuben Member
    edited December 2013
    I don't want to hijack the discussion, but I've seen so many offers over the internet of Vitamin C/Ferulic acid  serums and I wonder how they get around the patent issue. Are they too small and fly under the radar? or, they use less than 0.2% of ferulic acid or its derivative, which is the lowest concentration claimed by the patent.
  • MicroformulationMicroformulation Member, Professional Chemist
    https://www.google.com/patents/EP1742710B1?cl=en&dq=ferulic+acid+vitamin+c&hl=en&sa=X&ei=-Fm_UumYFNKEkQe6_oCgCQ&ved=0CEEQ6AEwAQ
    markfuller@microformulation.com Microformulation.com Microformulation Cosmetic Consulting provides Custom Formulations for both large Commercial accounts as well as smaller entrepreneurs. We can provide Naturally compliant Formulations under the NSF, NPA, Whole Foods and USDA Organic Certifications. BS.Pharm Albany College of Pharmacy, Union University.
  • RubenRuben Member
    I've read the patent. My question is how people/companies avoid infringing the patent.
  • MicroformulationMicroformulation Member, Professional Chemist
    They stay under the radar I believe. Perry has some experience with patents so he may be able to better respond.
    markfuller@microformulation.com Microformulation.com Microformulation Cosmetic Consulting provides Custom Formulations for both large Commercial accounts as well as smaller entrepreneurs. We can provide Naturally compliant Formulations under the NSF, NPA, Whole Foods and USDA Organic Certifications. BS.Pharm Albany College of Pharmacy, Union University.
  • PerryPerry Administrator, Professional Chemist
    Staying under the radar is one method.  It is up to patent holders to track down infringers if they want to collect damages.  As you can imagine, this could be costly.

    More reputable companies just use amounts of the ingredient outside the concentration range.
    Learn to formulate cosmetics
  • HerbnerdHerbnerd Member
    I had this problem recently with an Aloe Vera juice dietary supplement I developed for a customer. Everything looked fine on the shelf ( quickest way to see if anything goes wrong was to put on a shelf in bright sun... Mould shows up very quickly).
    Sent this away for preservative efficacy tests and 3/4 products came back fine. The fourth passed after a tweak to the preservatives.

    So, we felt fine to release for sale whilst doing on-going stability.

    Under accelerated stability the Vit C disappeared within hours in three of the four product. The fourth was still there but lower than the levels claimed.

    The difference between the fourth product and the others was addition of Vitamin E (dl-alpha tocopheryl acetate).

    The quickest solution to the problem was to add vitamin E to all products and increase the overage of the vitamin C by 120%. Ie 90 mg/serve claimed input amount was 198 mg/serve.

    Admittedly I was working with pharmaceuticals rather than cosmetics, but I am sure there will be a cross-over of information that could be useful. We did consider using Ferulic acid, but we wanted a solution that didn't require product relisting.
  • PerryPerry Administrator, Professional Chemist
    You started selling a product before you knew it was stable and possibly with a compromised preservative system?

    The lack of regulation in the dietary supplement industry in the US unsettling.  
    Learn to formulate cosmetics
  • DavidWDavidW Member, PCF student
    Barnet Products sells a stabilized form of vitamin C but I think it is oil soluble.  They refer to it as BV-OSC and it is Tetrahexyldecyl Ascorbate, CAS #: 183476-82-6


  • HerbnerdHerbnerd Member
    Hi Perry,

    I think I may not have been clear. We knew the preservation system was fine - that had been tested using preservative efficacy tests and 3 month accelerated stability to give 9 month shelf-life before the product went on sale. There has been on-going accelerated stability with each batch to ensure we can push this out to 36 months safely.

    We were tweaking the vitamin C levels based on the claims to ensure it could be assayed to the claim levels. This is normal practice under TGA (Australia) to conduct on-going stability to ensure compliance.

    I cannot comment on the US dietary supplement industry. There are different regulations to be dealt with.

    Under Australian Dietary Supplements regulations, they come under the same regs as pharmaceuticals and cosmetics and compliance is defined in law.
  • PerryPerry Administrator, Professional Chemist
    @Herbnerd - thanks for the clarification!  

    It's good to hear some countries take dietary supplement regulation seriously.  In the US, it's pretty much anything goes as long as no one can prove you've killed someone.
    Learn to formulate cosmetics
  • RubenRuben Member
    edited January 2014
    After Mark’s suggestion about using an anhydrous system to preserve vitamin c, I found this serum with vitamin c and caffeic acid that contain the following ingredients (I copied exactly as they were listed):

    Cyclomethicone (slip agent), Dimethicone Crosspolymer-3, Ascorbic acid (antioxidant), Dimethicone (slip agent), Bis-vinyl Dimethicone/Dimethicone Copolymer (slip agent), Tetrahexyldecyl Ascorbate (antioxidant), Tocopherol (antioxidant), Caffeic acid (antioxidant).

    I assume ascorbic acid and caffeic acid are not soluble in silicone at all, so I wonder how they were incorporated into the serum. Are they just in suspension?

  • Chemist77Chemist77 Member, PCF student
    Think either they have omitted something critical or as Robert generally says it is not a complete ing list. If the product is hazy and thick then they have simply suspended them into silicone gel.
  • alchemistalchemist Member
    The product will be just a suspension.  The silicones will be very good at keeping water & air out and nothing in there that the ascorbic acid will react with.
  • Chemist77Chemist77 Member, PCF student
    @alchemist Excellent point
  • RubenRuben Member
    I just found that they claim the ascorbic acid is "encapsulated" in dimethicone copolymer??
    Look down in the Comments section

  • pmapma Member
    edited January 2014
    Another form for vitamin C stabilization (in part of course) is doing a triple emulsion: W (with ascorbic acid)/Si/W. 
  • HerbnerdHerbnerd Member
    @pma - I read something about this a few months back. Using polyphase emulsions to stabilise vitamins in food.

    Can't quite remember the reason why they were doing this in foods though.
  • pmapma Member
    Here are two products that are triple emulsions to avoid vitamin C degradation:

    Aqua/Water/Eau, Glycerin, Cyclopentasiloxane, Ascorbic Acid (Vitamin C), Propylene Glycol, Nylon 12, Sodium Hydroxide, Citric Acid, PEG/PPG 18/18 Dimethicone, Disodium EDTA, Acrylates Crosspolymer, Isobutane, Methylparaben, Propylparaben, Parfum/Fragrance

    Water, Dimethicone, Iscocetyl Sterate, Glycerin, Mannose, Ascorbic Acid, Caprylic/Capric/Lauric TriglycerideButylene Glycol, Sucrose Tristearate, Potassium Hydroxide, Sodium Styrene/Ma Copolymer, Polymethylsilsesquioxane, Steareth-10, Madecassoside, Sodium Stearoyl Glutamate, Hydrogenated Lecithin, Hydrolyzed Hyaluronic Acid, Caprylyl Glycol, Tetrasodium EDTA, Acetyl Dipeptide 1 Cetyl Ester, Xanthan Gum, Acrylates Copolymer, Acrylates/C10-30 Alkyl Acrylate Crosspolymer, Phenoxyethanol, Fragrance

    Well, I suppose they are triple emulsions because they are from L'oréal and this company patented triple emulsions formulas for vitamin C.
  • Unknown Member
    edited June 2014
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  • simonasimona Member
    I wonder - those Ascorbic Acid products with no water- is there a special grind "type" I should be looking for when buying the vitamin, if I want to make it at home? The ascorbic acid I have is really gritty and I can't rub it against my skin if not solubilized.

    So, what type of AA should I search for, if I wanted to create a suspension in silicone ? which are the key words or, better, which should be the max particle size? 

    Can i also try to grind it at home (mortar/pestle or coffee grinder) to get a finer powder with no gritty feeling on the skin? 
  • vitalysvitalys Member
    I feel the strong doubt that any form of AA other than the pure acid would be effective on skin. It is the main issue related to this acid.
  • BobzchemistBobzchemist Member, PCF student
    Mortar and pestle won't work - it's more for plants. Use a muller:



    http://www.dullesglassandmirror.com/frosted-glass.aspx?gclid=CjkKEQjwrLSdBRDYvIL0soO4vo0BEiQABALkqfQD-7vQqF88KqSqvni6GVAs3gFGY8H7sPBzjLTHLmTw_wcB
    Robert Zonis, Sr. Formulation Chemist, Beaumont Products "All opinions and comments expressed are my own, have no relation to Beaumont Products, are fully copyrighted, and may not be used without written permission."
  • vitalysvitalys Member
    I recall we have learned the method of stabilization the Vit C in the Medical University and I have found it. So, you could try it. Stabilization ingredients are Sodium Sulfite with the presence of Sodium Bicarbonate.

    Here are the formulation:

    Ascorbic Acid -10.0%

    Sodium Sulfite -0.2%

    Sodium Bicarbonate - 4.7%

    Water - ad 100.0

    First the water should be boiled and cooled in a closed jar - it helps to rid the oxygen off the water.

    Then dissolve the sults and put the AA. Keep in a dry cool place in a dark glass container.

    Regularly they sterilize this solution. But I guess it would be presserved as well.

    Th pH of this stabilized solution should be 6-7 which is not bad for the skin as well.
  • johnsutwjohnsutw Member
    However,Pinnell claims that efficacy of l ascorbic acid in skin is pH dependent, less than pH3.5

    Source: Pinnell, S. R., Yang, H., Omar, M., Riviere, N. M., DeBuys, H. V.,
    Walker, L. C., Wang, Y. and Levine, M. (2001), Topical L-Ascorbic Acid:
    Percutaneous Absorption Studies. Dermatologic Surgery, 27: 137–142.
    doi: 10.1046/j.1524-4725.2001.00264.x
  • johnsutwjohnsutw Member
     'Philosophy' solved the stability issue by simply selling l ascorbic acid powder separately (' turbo booster c powder') and getting customers to mix it themselves with a water based serum or cream. Something many DIY skin care enthusiasts were doing well before Philosophy started selling their powder.
  • LaurannecarlyLaurannecarly Member
    Dears,

    Does anyone have any knowledge if it would be classified as patent infringement (of the CE Ferulic patent) when the formulation would be formulated at pH > 3.6? So the formula would contain 15% ascorbic acid, 1% vitamin E and 0.5% Ferulic acid at pH >3.6.

    Also, I am currently using 1% Tocopherol (natural mixed tocopherol) to stabilise the AA. Is Alpha Tocopherol better for stabilisation purposes vs. natural mixed Tocopherols (that include Alpha Tocopherol as well, but at a lower concentration)?

    Finally, what is the best pH adjuster when working with high concentrations of Ascorbic acid. I notice that the moment any pH adjuster is added, the degradation of AA occurs more quickly. Would Sodium hydroxide (20% solution) be a suitable option? Or would other pH adjusters be better to avoid negatively impacting AA stability?

    Many thanks in advance!
  • DtdangDtdang Member
    Use ethyl ascorbic, the stable form of vitamin C. Easy to formulate 


  • DtdangDtdang Member
    Another points;
    vitamin C needs pH of 3.5 for effective 
    other stable form of C needs pH of 5 to 6
  • EVchemEVchem Member
    edited January 2020
    @simona ; if this site ships to you https://lotioncrafter.com/products/l-ascorbic-acid-ultrafine?_pos=1&_sid=6fa9b20b5&_ss=r

    About every 6 months we get a request to copy skinceuticals and we have to explain to sales it is patented and the  options around it. I think higher pH is the easiest  work around, but  like others are saying i don't think it's helping product efficacy. You can always try the derivatives, my personal favorites are ascorbyl glucoside and the amitose series from seiwa (though those are more for feel than true efficacy)

    I think most places do stay under the radar, but if your product gets popular they are more likely to come after you...'because you're worth it' (sorry can't resist)
    https://www.thefashionlaw.com/home/loreal-is-suing-drunk-elephant-for-patent-infringement-over-its-buzzy-vitamin-c-serum
  • DtdangDtdang Member
    @EVchem , the pure vitamin C has pH < 2.5 . That means the skin can be irritated? We have to use NaOH to bring pH to > 3.5
    with pH > 3.5 the vitamin C still effective?
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