Raw material -> first cosmetic product. Assurance for industry novice to not go wrong way.

Hi everyone, i am new to this awesome forum and here comes my first and long post.

First of all i would like to tell that i do not have chemistry or cosmetic background and i got into the cosmetic industry by very lucky coincidence  about 6 months ago.

Since then i have been only raw material supplier to some specific companies.

About a month ago i thought i will try to make my own cosmetic product ( face mask) since i really like the material i have under my possession.

Basically my product is sea mud/silt/clay ( minerals 94%, organics 5%, carbonates 1% ) with a PH of 6.8-7.2. Dry matter 35%, water 65%. INCI name Maris Limus. 

I quickly ran microbiological TVC test with my base material in its natural state and the results for microbial bacteria count was 30 000cfu/g ( 3x10’3). So i figured there might not be too much of a excessive work to get microbial bacteria count compatibility under the EU Cosmetic law (category 2). 

After a few days in Google and cosmetic forums i ordered ~10 different preservatives which i thought would work with my high PH and be cost efficcient, yet still marketable to nowadays greenheads/diletants in their anti-paraben, formaldehyde etc madness. Made multiple different samples with different preservatives and after 2 days of waiting i took them all to the State laboratory for testing. 

Some of the results are listed below:

99% Maris Limus + 1% Geogard 221 ( Dehydroacetatic acid 8%, Benzyl Alcohol 88%, Aqua 4% ) = 460 cfu/g

99% Maris Limus + 1% Plantaserv E ( Phenoxyehtanol 90%, Ethylhexylglycerin 10% ) = 250 cfu/g

99% Maris Limus + 1% Chemikons ( 2-phenoxyethanol, Ethylhexyglycerin ) = 630 cfu/g

99% Maris Limus + 1% Phenoxyethanol = 740 cfu/g

96% Maris Limus + 4% Dermosoft OMP ( Methylpropanediol, Caprylyl Glycol, Phenylpropanol ) = 530 cfu/g

96% Maris Limus + 4% Dermosoft OMP + 1,5% Ecogel ( Lysolecithin, Sclerotium Gum, Xantham Gum, Pullulan) = 130 cfu/g

There were some preservative reaction results over 1000 cfu/g and some that did not react at all ( probably too low PH range ) .

As you can see with those bolded results i can really move on with my cosmetic product registration but i still have some questions to which i can not answer on my own at the moment that quickly. My inner gut told me to ask from industry experts in here. So...

Am i being too naive to think that if i mix my material with preservative which acts as a bactericide at first and then afterwards keeps the material clean from possible contamination, then it is just like that for the rest of the 30 months which i am planning to be best before ? Or is it naive and bacteria will start growing soon after ?

Secondly i have problems with my product odour/scent/smell after mixing it with preservative. It all smells like one big preservative. Can you give me some hint where i can search something or recommend me some ingredients to add into the mix to get rid of the unwanted preservative odour ? Or add some extra perfume ?

Also i did not use any emulsifier exept one sample, since i do not know for sure that i have to use one. I only could find one cold processable emulsifier with the PH working range ~7.

Can anyone tell for novice like me, should i use any emulsifier ? Does it mix preservative better with my material ? Should i use some other ingredient in order to work my preservative better or to be more ensured that my product will stay the same for 30 months ?

Sorry for making such a long post, but i really wanted to paint the bigger picutre in order to get a real help if somebody would really like to help me :smile:

Many thanks if someone will answer at least some of the questions!

Karel

Comments

  • I will leave this to others with more knowledge of the sector, but I just wanted to say that you are on exactly the right track by doing all your experiments and as a result you have already learned a lot about your materials and the effectiveness of the preservatives, and thanks for sharing this useful information with us.
    Design of anti-aging creams, gels, and serums; shampoos; and therapeutic cosmetics. In-house label and box design capability.
  • Disclaimer, I am not an expert however can adress one thing here. Most of your preservatives contain phenoxyethanol. It has a strong smell. That was one of the
     reasons why I switched to parabens. I don’t say parabens don’t have any smell at all, but definitely better than phenoxyethanol. Also I think you need a chelating agent to boost preservative’s efficacy, but experts should confirm.
  • A chelating agent would be overwhelmed by clay.
    Design of anti-aging creams, gels, and serums; shampoos; and therapeutic cosmetics. In-house label and box design capability.
  • Thank you both for the responses.

    I can see that there have not been any other opinions on my issue but i am still  fighting to get there by myself aswell;)

    Belassi, what do you mean by saying chelating agent would be overwhelmed by clay ? That it is pointlss to use with clay ? 

    As i understand chelating agent for example sodium phytate / phytate acid will bind up metal ions to not let bad microbes into them ? 

    Or have i misunderstood something ? 
  • what do you mean by saying chelating agent would be overwhelmed by clay ?
    There will be so many metal ions in the clay. 
    Content in % 20 SiO2 15.5 CaO 4.8 Al2O3 4.5 MgO 2.8 Fe2O3 1.7 Na2O 1.3 K2O 0.5 TiO2 0.4 SO3 0.3 P2O5 6.7 Cl 0.2 Br
     Content in PPM Trace elements 550 Sr 250 Mn 200 Ba 75 Cr 60 Zn 60 V 40 Ni 25 Li 20 Cu 8 Co 4 Pb 3 Th 2 As 2 U 2 Mo 1 Sn < 1 Ag 0.7 Be 0.6 Cd 0.2 Sb
    Design of anti-aging creams, gels, and serums; shampoos; and therapeutic cosmetics. In-house label and box design capability.
  • Ok

    So in order to get an effect of chelating agent itself, i should use so much of it that it would be pointless to use one, do i understand correctly ? 
  • Exactly.
    Design of anti-aging creams, gels, and serums; shampoos; and therapeutic cosmetics. In-house label and box design capability.
  • edited October 8
    I know by my quite limited experience that it might be very challenging to preserve clay. May be you want to consider making a powder product? I assume your raw material is powder?
  • @NoviceKarel
    What about boiling the maris limus before using to kill existing bacteria?
    Being mostly mud, I don't think it will degrade, although drying it might be time consuming.

    Parabens are approved by the EU up to certain concentrations
    if I'm not mistaken
    methylparaben 0.4%
    propylparaben 0.19%
    Maybe stating that your product meets European safety specs will calm your customers down (be careful with european fragance INCI naming regs).


    @ngarayeva001 do parabens have a smell?
    Maybe just smelling the raw powder, but not when diluted to use.
    Also, paraben Sodium salts have virtually no smell.
  • @Gunther You're not mistaken, however, it's 0.4% as acid for PHBA, Methyl- and Ethylparaben and their Na, K and Ca salts.

    And 0.14% for propyl- and butylparaben and their Na & K salts (as acid)

    0.8% in total (as acid) for combinations of esters where the sum of the individual concentrations of butyl- and propylparaben and their salts does not exceed 0.14 %

    The limitations are written in the annex here:


    Dabbling Formulator — Qualified Cosmetic Safety Assessor — experienced in claim substantiation & EU regulatory affairs.
  • I have nothing to say about the preservative side of things (other than this information you have provided is valuable), but if you want to fragrance your formulas "naturally" you can try Aromatic Waters or Aromatic Extracts. We get ours from Carrubba.They are also kind of pricey so that might not be a viable option, but still throwing it out there. 
  • Thank you gld010 for good option!
    I will look it up.

    Yesterday i ordered different types of high scent fragrance oils. For example coconut fragrance oil ( DIETHYL PHTHALATE + COUMARIN ).

    We'll see how adding this affects overall scent outcome. Although even if it works then there might occur problem with COUMARIN which gets 7 out 10 points in the hazardous scala in ewg database.

    Parabens are unfortunately out of the question at the moment because of the green/natural madness. 

    I do not make my product out of powder. I have the license to excavate very very high quality sea mud from the natural reserves which makes it being very pure and the material is in its natural state like i described above.

    I have made powder version of it aswell by drying my regular wet product but only with the raw material selling purposes, not for my own cosmetic product purposes.

    Big thanks for everyone trying to help, really aprecciate it !
  • @Gunther parabens (at least the blend that I am using ) have a subtle ‘chemical’ smell. But it’s nothing in comparison to phenoxyethanol.

    @NoviceKarel, EWG database isn’t the most reliable source. A lot of scaremongering without scientific proof.
  • edited October 11
    @ngarayeva001
    You're sure your phenoxyethanol isn't in a blend? My pure phenoxyethanol has a slight flowery scent, I like it. The worst smelling blend for me was Geogard 221. I like the smell of benzyl alcohol, but the dehydroacetic acid made it just plain terrible.
  • @Doreen, I have two versions, one is mixed with sorbic acid and caprylyl glycol, another with ethylhexylglycerin. Both have very similar strong "chemical" smell. 
  • Scent of pure phenoxyethanol and scent of phenoxyethanol in different blends is pretty much the same and yes it seems pretty "chemical scent" . At least for my nose sensors...

    Geogard 221 blend reminds me a little bit of marzipan scent, but unfortunately it is still too strong to be pleased with it. 
  • I guess it's personal then. Pure phenoxyethanol, just like benzyl alcohol and phenethyl alcohol, have a flowery scent to me. Can't say I dislike it. ❁
  • Just to be sure that i do not own any rancid version of phenoxyethanol, i will order it once again.
  • get your clay sterilised, preferably by irradiation - it's the most likely vector for contamination and if it's clean to start with, your microbial count will be much lower

    (also, minor pedantry: 30,000 = 3 x 10^4, not 3 x 10^3)
    UK based formulation chemist. Strongest subjects: hair styling, hair bleaches, hair dyes (oxidative and non-oxidative) I know some stuff about: EU regulations, emulsions (O/W and W/O), toothpaste, mouthwash, shampoos, other toiletries
  • You need to use sterilsied caly,
    Second thing there are many natural preservative are available that you have try and may be you have to used two to four preservative in combination to control the microbs.

    I made lost of masks and we had used three to four preservatives in combination.

    Ideally Microbs must be <10 is better.
  • edited October 12
    @Bill_Toge
    About the scents mentioned in this thread.
    I was just enjoying a thread named 'best and worst smelling chemicals' on a science forum, when I read the reply of a forum member that wondered (and I quote): "What in the unholy hell is the smell that comes off of sodium hydrosulfite in solution. It's abominable and more vile than hydrogen sulfide alone. "

    I had to think of you and your 'tub of death' nickname. :joy: :joy: 
    I nearly fell on the floor laughing when I read a possible answer (several sulphurous compounds that are formed in your nose) and experiences from other members. (gag inducing Taco Bell fart smell)  :D

    @NoviceKarel
    My excuses for being off topic with this, but I just had to share it.
    Even phenoxyethanol gone rancid can't be thát bad. :wink: 
  • @Doreen, talking about terrible smells, nothing is worse for me than silk amino acids. Phenoxyethanol really smells like flowers comparing to it.
  • @ngarayeva001
    I never use proteins no more because of the terrible smell, no matter it's from oat, wheat or silk... it's just disgusting! :no_mouth:
  • @Doreen have you tried oat silk? It’s simply oats flour. It’s ok for ‘claims’ doesn’t mess up rheology and has a neuthal smell. I agree proteins smell terrible. I don’t know what to do with that bag of silk, I don’t even use fragrances to hide that smell 😂
  • edited October 26
    @ngarayeva001
    I have used oatmeal quite often in moisturizers in the past, around 2-2.5%. Because it's such a challenge to preserve as it's bugfood, I make freshly made masks with it and leave it on the skin for a while for the soothing effect.
    You're right, it's nearly impossible to hide the smell of proteins, it's still a vomit-like (and inducing) smell combined with a fragrance. :persevere:

    @NoviceKarel
    Did you order a new batch of phenoxyethanol and did it smell differently?
  • Anyone familiar with silk peptides?  Thinking of what would be the best product to incorporate them into. 
  • @Jdawgswife76 I regret buying them. I tried to incorporate them in hair conditioner. The smell  was unbearable.
  • I have made face mask formulations which are quite good, and once played with incorporating a natural source substance found in some banks of underground streams.  But, I ran into the bacterial elimination problem and ended up using commercially available sterilized clays. 

    The relevant information as relates to your situation is that your access to the natural material might not be as good fortune as you envision.  You would need to start out with a sterilized clay base and sterilizing that material with an appropriate heating situation (oven) may cause changes in its properties that would make it unsuitable.  An option other than heat is radiation. I found two places, one in Canada and another in Texas.  You can Google for places which will do that for you. I have tested them for other applications and they are amazing in their completed sterilization of plant origin materials which are loaded with bacterial substances and other organisms in their supplied state. Sterilized clays are readily available.  So, that might be your best option.

    As far preservatives, you might want to experiment with Optiphen Plus. It's made by Ashland Chemical. It now has global approval and it is paraben-free and formaldehyde-free.  It meets modern market expectations for a preservative system,
  • @Doreen
    Yes, I have received a new patch of phenoxyethanol and the scent outcome remains, unfortunately, the same.

    @perspicacious
    It is encountering to hear that there are more people experiencing difficulties with the bacterial elimination from fully natural material.
    Bypassing excitement is slowly replaced with the actual knowledge of the material itself and therefore I can say that there truly are multiple factors affecting the outcomes of different testings. Lots of characteristics to consider working with the material.

    It is overwhelming to hear that you end up mentioning radiation since this week I ordered sterilization tests with my material through 10 kGy gamma radiation ( Cobalt 60 isotope ). Of course, it is expensive and pretty bad market-wise for dilettants but the actual effect of it should be outstanding considering the situation with my complex, yet good and natural material.
    At least i think and hope so.

    Offtopic:

    Have anyone had experience with the registration of cosmetic product which has been sterilized through gamma radiation? ( Haven't had time to check it's compatibility with the EU cosmetic law, does the manufacturer have any duties of informing the customer about sterilization process?...)

    I will let you know about the outcome of tests!

    Thanks for everyone 
  • Can you buy directly from Shulke 9010, it comes with ethylhexylglycerin and I have never had a problem with odour. Hope this helps
    Dr. Catherine Pratt
    (B.Sc with HONS I , Ph.D Analytical/Organic Chem and Microbiology), Cosmetic Chemistry IPCS)
  • Can you buy directly from Shulke 9010, it comes with ethylhexylglycerin and I have never had a problem with odour. Hope this helps
    Neither have I, I kinda like the scent! But I'm afraid if you don't like the smell of phenoxy, you're not going to like Euxyl PE 9010 either.
  • Doreen, I just had a smell and I cannot smell anything???
    Dr. Catherine Pratt
    (B.Sc with HONS I , Ph.D Analytical/Organic Chem and Microbiology), Cosmetic Chemistry IPCS)
  • Honestly, at the levels used, Euxyl PE9010 has little to no influence on the final fragrance in the finished product. Ensuring that a chelant is used and being aware that it can destabilize an emulsion are the biggest concerns.

    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.
  • Yes I agree, plus you need to get some practice at masking bad odours, or no-one would wash, use make-up or brush their teeth!
    Dr. Catherine Pratt
    (B.Sc with HONS I , Ph.D Analytical/Organic Chem and Microbiology), Cosmetic Chemistry IPCS)
  • Doreen, I just had a smell and I cannot smell anything???
    I smell a slight rose-like floral scent. There are some members here (older posts in this thread) who absolutely dislike the smell and describe it otherwise.

    Honestly, at the levels used, Euxyl PE9010 has little to no influence on the final fragrance in the finished product. Ensuring that a chelant is used and being aware that it can destabilize an emulsion are the biggest concerns.

    I think so too. Even in a fragrance free formula with 1% Euxyl PE9010.
  • @Jdawgswife76 I regret buying them. I tried to incorporate them in hair conditioner. The smell  
  • @ngarayeva001 the silk smells peptides smell bad or just in the conditioner?  Im thinking of the powder and conditioner would be the fist place i would look to put them but not if they stink. 
  • edited November 18
    @Jdawgswife76
    The smell is there in any formula, depending on %.
    I found it hard to mask with fragrance in the recommended %.
    You could use it as claims ingredient at 0.1%, or so?
  • So i have ran into a preserving issue with making clay masks with kaolin,  indian healing,  Moroccan,  and french green as well as black charcoal.  Anyone have any suggestions on a good preservative for these for a good shelf life? 
  • I really dislike smell of phenoxyethanol. @Jdawgswife76, it’s very difficult to preserve clay based product. It deactivates phenoxyethanol and some other preservatives. I recently bought phenonip, it’s phenoxyethanol and a mix of several parabens. Should be a very strong preservative, but haven’t tested yet.
  • Can you lmk how it works out for you using that preservation system?  Im really wanting to make up and package some masks but of course want to be sure they are very well preserved. 
  • Also with the silk i have the powder and not the peptides.  Is that what has the bad smell?  The peptide? 
  • @ngarayeva001 the silk smells peptides smell bad or just in the conditioner?  Im thinking of the powder and conditioner would be the fist place i would look to put them but not if they stink. 
    Would the powder smell the same way you  think?  The powder has great benefits for the skin and is great in creams,  powders,  foundations,  etc but i have never noticed a smell of any kind from the powder i have. 
  • @Jdawgswife76 what is INCI of the product you are using? It should be some type of protein (amino acids, peptides) to have skin benefits (not really proven) and proteins often have horrible smell. Also proteins compromise viscosity of certain polymers. I recommend you to start a new topic about benefits of silk. Let’s see what professionals think and is there any proof that silk even does anything for skin.
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