Home Cosmetic Science Talk Formulating Glycol and Chelating Agents

  • PhilGeis

    Member
    July 19, 2022 at 12:23 pm

    Just phenoxyethanol.  That is a poor system.  You’ve nothing to address fungi.  Please understand, merely passing a challenge test is not enough - such tests are not validated to anything.
    You should design a system vs bacteria and fungi and then test to confirm expected efficacy.

  • Newtoformulating

    Member
    July 21, 2022 at 1:05 am

    @Fekher Thanks for the words of encouragement! The final texture is a like that of a creamy peanut butter. Not waxy or oily. The final hold is a soft firm hold. It’s not a crunchy hold like I experienced using PVP

    @evchem2 yes I do understand what you are saying and will evaluate my formula again because if an ingredient is not needed then I won’t include it. Thanks for your response and helping me with critical thinking and reevaluating my formula!

    @MariaSibon definitely reevaluate your preservation system! When I used Optiphen Plus (Phenoxyethanol, Caprylyl Glycol, and Sorbic Acid)
    my system was WEAK! I’m looking now to build a stronger preservation system and also using preservative boosters to make my system even stronger. I too had an issue at 1 month post accelerated conditions where my sample turned white from clear with no explanation. I’m still puzzled as to what happened but I’m almost certain the preservative I was using (Optiphen plus) was the issue. My pH wasn’t affected just the clarity. See photo.

  • MariaSibon

    Member
    September 5, 2022 at 11:11 am

    PhilGeis said:

    Just phenoxyethanol.  That is a poor system.  You’ve nothing to address fungi.  Please understand, merely passing a challenge test is not enough - such tests are not validated to anything.
    You should design a system vs bacteria and fungi and then test to confirm expected efficacy.

    @PhilGeis

    Thank you for your comment.

    Apologies I missed to mention the preservative is a mixture of phenoxyethanol 0.9% , glyceryl laurate 0.1%, the second as an adsorption enhancer boosts phenopxyethanol efficancy to microorganisms. 
    Also I forgot to mention I use colourants to the formulation which I think this causes the stability issues to my formula as it fades away in 2 months accelerated condition in a black packing.

    Why you think a challenge test is not enough? The challenge test performed was as per ISO 11930, that include 5 microrganisms (3 bacteria, 2 fungi).
    I also have a control sample that 18 month micro analysis was clean versus all those microorganisms.

    My preservative may not be the strongest in the market but do I need a stronger one if I have these results? Also taking into account the nature of the product consisting of 30% of a surfactant and allowing low water activity due to its physical state I would consider it a rather low risk contamination product. That is why I do not think my stabilities issues has to do with the preservation system, but with my ingredients. Open to your suggestions, thank you.

  • PhilGeis

    Member
    September 5, 2022 at 11:43 am

    Not aware Glycerol laurate adds anything preservation.   Perhaps if hydrolyzed by bacterial esterase, the laurate would have an effect.  You need a preservative that addresses fungi and works better vs Gram + bacteria.  As a surfactant based product - use Na benzoate ~3000 ppm, it covers those gaps and actually boosts vs. Gram neg.

    The test (USP, BP, EP, or11930) is not validated to any endpoint - not manufacturing or consumer contamination.  These are modifications of a test developed last century for drug preservation - using largely clinical (not industrial)isolates also from last century - one is almost 100 years from isolation and the most recent ~ 60 years  and from a blueberry.  
    Every recall you see on FDA’s enforcement reports passed this kind of test.  One should design a system that should be broadly effective and confirm general efficacy with one of these tests.

    Please consider the product - not just the formula - in estimating risk.  Surfactant based cosmetics (shampoos, body washes, liq. hand soaps) typically suffer water intrusion in use and are prob the most commonly contaminated in use.   to that - what is the quality of your process water?
    What is Aw?  Be aware that this not limiting - even liquid laundry detergents have significant contamination problems.  

  • MariaSibon

    Member
    September 5, 2022 at 12:33 pm

    @Fekher Thanks for the words of encouragement! The final texture is a like that of a creamy peanut butter. Not waxy or oily. The final hold is a soft firm hold. It’s not a crunchy hold like I experienced using PVP

    @evchem2 yes I do understand what you are saying and will evaluate my formula again because if an ingredient is not needed then I won’t include it. Thanks for your response and helping me with critical thinking and reevaluating my formula!

    @MariaSibon definitely reevaluate your preservation system! When I used Optiphen Plus (Phenoxyethanol, Caprylyl Glycol, and Sorbic Acid)
    my system was WEAK! I’m looking now to build a stronger preservation system and also using preservative boosters to make my system even stronger. I too had an issue at 1 month post accelerated conditions where my sample turned white from clear with no explanation. I’m still puzzled as to what happened but I’m almost certain the preservative I was using (Optiphen plus) was the issue. My pH wasn’t affected just the clarity. See photo.

    @Newtoformulating

    Thank you for your comment.
    As I explain below, I was not worried for the preservation system as my challenge test and 18 months micro was clean. I may be wrong of course, still researching that.
    In my case I think is the degradation of the colourant upon other ingredient with the heat effect. But I still research, that is why I asked and I am open to opinions.

    It may be your preservative, but not from the point of view of preservation efficacy, but rather stability/chemical interaction with the other ingredients.

    I dont think it is a good idea to have sorbic acid in your preservative mixture and have a neutral or higher ph, as it looses its effect. Also since your are using acrylates copolymer/AMP system, you will never manage to have an acidic pH, as the acrylates copolymer will loose its function. 
    My guess is that the cloudiness in your product is a reaction of sorbic acid with AMP, that created the respective salt. Do a test and lower the pH <6. The viscosity will change, but does it become less cloudy?

    Did you have this reaction also with other phenoxyethanol mixtures without sorbic acid?

  • PhilGeis

    Member
    September 5, 2022 at 1:17 pm

    What is complete formula?  Any protein?

  • ketchito

    Member
    September 6, 2022 at 1:37 pm

    @Newtoformulating If you heat your product and it turns clear again, it might be due to the kraft point of your system. Perhaps you could remove Ceteareth-25 (which is waxy) and increase your PEG-40 HCO if needed.

  • Newtoformulating

    Member
    September 7, 2022 at 1:56 pm

    @Fekher Thanks for the words of encouragement! The final texture is a like that of a creamy peanut butter. Not waxy or oily. The final hold is a soft firm hold. It’s not a crunchy hold like I experienced using PVP

    @evchem2 yes I do understand what you are saying and will evaluate my formula again because if an ingredient is not needed then I won’t include it. Thanks for your response and helping me with critical thinking and reevaluating my formula!

    @MariaSibon definitely reevaluate your preservation system! When I used Optiphen Plus (Phenoxyethanol, Caprylyl Glycol, and Sorbic Acid)
    my system was WEAK! I’m looking now to build a stronger preservation system and also using preservative boosters to make my system even stronger. I too had an issue at 1 month post accelerated conditions where my sample turned white from clear with no explanation. I’m still puzzled as to what happened but I’m almost certain the preservative I was using (Optiphen plus) was the issue. My pH wasn’t affected just the clarity. See photo.

    @Newtoformulating

    Thank you for your comment.
    As I explain below, I was not worried for the preservation system as my challenge test and 18 months micro was clean. I may be wrong of course, still researching that.
    In my case I think is the degradation of the colourant upon other ingredient with the heat effect. But I still research, that is why I asked and I am open to opinions.

    It may be your preservative, but not from the point of view of preservation efficacy, but rather stability/chemical interaction with the other ingredients.

    I dont think it is a good idea to have sorbic acid in your preservative mixture and have a neutral or higher ph, as it looses its effect. Also since your are using acrylates copolymer/AMP system, you will never manage to have an acidic pH, as the acrylates copolymer will loose its function. 
    My guess is that the cloudiness in your product is a reaction of sorbic acid with AMP, that created the respective salt. Do a test and lower the pH <6. The viscosity will change, but does it become less cloudy?

    Did you have this reaction also with other phenoxyethanol mixtures without sorbic acid?

    I’m not sure as I’ve discontinued all Phenoxyethanol use. I did conclude that it may have been the sorbic acid reacting to another ingredient but didn’t dig deep enough to see which one. Your theory that the sorbic acid reacted with the AMP makes sense to me. I’ve since switched to Euxyl k940 as a preservative and will play around with my formulation a little more today. Yes I did realize I used the wrong preservative as opposed to my higher pH level. Euxyl k940 is more pH friendly to my formulation. I am now having an issue with dissolving ceteareth-25 in water. I’ve dissolved it separately in the oil phase and heated the water and oil phases to the same temp and mixed them together only for the ceteareth-25 to clump up and I’ve also put water and ceteareth-25 in the same vessel, heated and dissolved them together but the ceteareth-25 never completely dissolved. It may be because I’m using it at 23% of my formula but any lower percent the end formulation will not become solid. So any suggestions that way will be much appreciated. Also, do you think there is an issue with my pH being close to 7 with a hair gel product? I know that’s not a typical pH for this type of hair product but there’s really no way around it with the acrylates copolymer and AMP system that Im using. Thank you and please keep me posted on your research with your formula and your findings.

  • Newtoformulating

    Member
    September 7, 2022 at 2:02 pm

    ketchito said:

    @Newtoformulating If you heat your product and it turns clear again, it might be due to the kraft point of your system. Perhaps you could remove Ceteareth-25 (which is waxy) and increase your PEG-40 HCO if needed.

    The sample is at the lab so I would have no way of knowing that but could you explain what you mean kraft point? Since my sample did turn cloudy dies that necessarily mean there is an issue with my formulation or could it be something that is expected to happen if it is heated excessively? Also if I remove the ceteareth-25 what would you suggest replacing it with? Thanks!

  • PhilGeis

    Member
    September 7, 2022 at 2:42 pm

    @Newtoformulating
    Euxyl K940 is phenoxyethanol - with benzyl alcohol and EHG.

  • Newtoformulating

    Member
    September 8, 2022 at 3:46 am

    PhilGeis said:

    @Newtoformulating
    Euxyl K940 is phenoxyethanol - with benzyl alcohol and EHG.

    You are so right! I’ve played around with so many preservatives to find the one that works best for my formula and my wires are all mixed up! Thanks for correcting that! Still using Phenoxyethanol just not the Optiphen preservatives…..

  • PhilGeis

    Member
    September 13, 2022 at 10:53 am

    @Newtoformulating
    I understand.  Preservative marketing is a pain.  So many combinations with similar names, many of which are +/- useless.

  • MariaSibon

    Member
    October 25, 2022 at 7:10 am

    @Fekher Thanks for the words of encouragement! The final texture is a like that of a creamy peanut butter. Not waxy or oily. The final hold is a soft firm hold. It’s not a crunchy hold like I experienced using PVP

    @evchem2 yes I do understand what you are saying and will evaluate my formula again because if an ingredient is not needed then I won’t include it. Thanks for your response and helping me with critical thinking and reevaluating my formula!

    @MariaSibon definitely reevaluate your preservation system! When I used Optiphen Plus (Phenoxyethanol, Caprylyl Glycol, and Sorbic Acid)
    my system was WEAK! I’m looking now to build a stronger preservation system and also using preservative boosters to make my system even stronger. I too had an issue at 1 month post accelerated conditions where my sample turned white from clear with no explanation. I’m still puzzled as to what happened but I’m almost certain the preservative I was using (Optiphen plus) was the issue. My pH wasn’t affected just the clarity. See photo.

    @Newtoformulating

    Thank you for your comment.
    As I explain below, I was not worried for the preservation system as my challenge test and 18 months micro was clean. I may be wrong of course, still researching that.
    In my case I think is the degradation of the colourant upon other ingredient with the heat effect. But I still research, that is why I asked and I am open to opinions.

    It may be your preservative, but not from the point of view of preservation efficacy, but rather stability/chemical interaction with the other ingredients.

    I dont think it is a good idea to have sorbic acid in your preservative mixture and have a neutral or higher ph, as it looses its effect. Also since your are using acrylates copolymer/AMP system, you will never manage to have an acidic pH, as the acrylates copolymer will loose its function. 
    My guess is that the cloudiness in your product is a reaction of sorbic acid with AMP, that created the respective salt. Do a test and lower the pH <6. The viscosity will change, but does it become less cloudy?

    Did you have this reaction also with other phenoxyethanol mixtures without sorbic acid?

    I’m not sure as I’ve discontinued all Phenoxyethanol use. I did conclude that it may have been the sorbic acid reacting to another ingredient but didn’t dig deep enough to see which one. Your theory that the sorbic acid reacted with the AMP makes sense to me. I’ve since switched to Euxyl k940 as a preservative and will play around with my formulation a little more today. Yes I did realize I used the wrong preservative as opposed to my higher pH level. Euxyl k940 is more pH friendly to my formulation. I am now having an issue with dissolving ceteareth-25 in water. I’ve dissolved it separately in the oil phase and heated the water and oil phases to the same temp and mixed them together only for the ceteareth-25 to clump up and I’ve also put water and ceteareth-25 in the same vessel, heated and dissolved them together but the ceteareth-25 never completely dissolved. It may be because I’m using it at 23% of my formula but any lower percent the end formulation will not become solid. So any suggestions that way will be much appreciated. Also, do you think there is an issue with my pH being close to 7 with a hair gel product? I know that’s not a typical pH for this type of hair product but there’s really no way around it with the acrylates copolymer and AMP system that Im using. Thank you and please keep me posted on your research with your formula and your findings.

    Hello, apologies I missed this discussion.
    I hope you already managed to solve your problems.
    regarding Ceteraeth-25 solubility to water, you just need to use high temperature up to 85 C. I use upo to 30% in some formulations with no issue.
    No issue this product at ph 7, I believe as this is the only cases for many styling products based on carbomer thickeners. 

    If you want to make your pH lower and use other preservation system, just get read of Acudyne 1000, fixative function can be succeed only with high concentrations of your “surfactant gel”.

    DId Euxyl k940 worked well for you? 
    In my trials I conclude that instabilities occur most probably due to the colourant I use. Addition of EDTA in my formula seems to help.

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