Odor masking/neutralizing AFTER batch completion

Hi all,

I was hoping to get some insight and tips/tricks on a batch issue I am facing at the moment. A new moisturizer project I have been working on has gone through multiple iterations and tweaks to come to a final approved formula. From lab samples to the pilot batch, there was no discernible smell at all. A rather neutral aroma, if anything. Well, we just batched a larger 150kG run and bottled some of it for a clinical trial, and there is now a distinct odor that I can only describe as oyster-like, briny, sea smell, etc. It dissipates about 5+ minutes after skin application, but that initial aroma is, at least in my opinion, not pleasant.

Outside of scratching my head trying to figure out why/how this happened, I now need to figure out how to fix this batch, if even possible after the fact. My goal is to avoid a Fragrance INCI, mostly for consumer perception with our target clientele. I have used aromatic preservatives in the past, like Dermosoft OMP, and when formulating with it from the beginning it provides a pretty delicate and pleasant aroma. However, adding it to this specific batch after the fact, and it's not really achieving the objective as it almost changes the profile altogether. I have ordered samples of some other options in the Dermosoft family to see if they can help. I have has also reached out to Ashland and Wacker to get some insight and if their cyclodextrin materials could assist in this situation. 

I have never encountered this in all my years formulating. Off smells have been discovered and fixed early on, way before bulk batching. So this one is rather perplexing! I thought I would try and get some insight from you all, see if you have some ideas or have encountered this before, and hopefully discover some viable options. Some members of my team have said it's "not that bad", but I take pride in my formulas and don't really want to release this as a first impression on the market. Ideally, I would love to save the 150 kilos and not toss it. I appreciate the help and insight. The formula, skin feel, and texture are fantastic, I just need that odor gone. Is this a hopeless case? 

For some specifics:
O/W emulsion
12% lipid phase with a blend of plant oils and CCT
Tocopherol to protect
Geogard 221
(anything else, just ask and I can provide)

Thank you.
Matt

Comments

  • DavidDavid Member
    The formulation would help.
  • @David you bet. 

    None of these materials present with an off odor individually, and when combined into the final formula, every batch has come out fine/neutral. It is just this recent 150 kg batch. If you need more specifics just let me know. I appreciate it. 

    Water (Aqua), Caprylic/Capric Triglyceride, Carthamus Tinctorius (Safflower) Seed Oil, Glycerin, Actinidia Chinensis (Kiwi) Seed Oil, C12-16 Alcohols, Inulin, Xylitylglucoside, Ectoin, Glyceryl Stearate, Palmitic Acid, Hydrogenated Lecithin, Saccharide Isomerate, Tasmannia Lanceolata Fruit/Leaf Extract, Terminalia Ferdinandiana Fruit Extract, Cholesterol, Glucosyl Ceramide, Phospholipids, Anhydroxylitol, Xylitol, Tocopherol, Glucose, Phytic Acid, Citric Acid, Sodium Citrate, Sodium Hydroxide, Xanthan Gum, sh-Oligopeptide-1, sh-Oligopeptide-2, sh-Polypeptide-31, sh-Polypeptide-5, sh-Polypeptide-10, sh-Polypeptide-11, sh-Polypeptide-1, sh-Polypeptide-6, Benzyl Alcohol, Dehydroacetic Acid

  • DavidDavid Member
    edited October 8
    Unless you have overseen some raw material differences when scaling up, the usual suspect is processing time. Warming /Cooling and mixing 150kg takes much longer time than 150g which gives more time for unwanted chemical reactions to take place. 
  • @David very good points. Thanks for that insight. Hopefully, I can come up with a temporary solution for this batch, and modify processing on the next one. Thanks again!
  • PharmaPharma Member, Pharmacist
    What's the pH of your product?
    Judging by your description of the smell and your LOI, I would guess that some of the peptides have deteriorated either forming amines (less likely) or reacting with sugars (Maillard reactions). Maillard reactions are most likely because you have peptides and ectoin alongside glucose and a bunch of oligosaccharides and plant extracts in your formulation. In the former case (free amines), dropping pH can help, in the latter case, a large trash can would be the way to go. Many Maillard products are potent aroma chemicals which will be very difficult to mask unless you add a flavour. Alas, this won't reanimate any potential physiological effect of the degraded 'actives'.
    The main reason for such Maillard reactions is, as @David mentioned, heat or in this case how long you heat.
    Either try a cold process or add all the critical ingredients after full cool down.
  • @MattTheChemist Considering that your product has a pH low enough for your DHA to work, I honestly don't know how Benzyl alcohl and Dehydroacetic Acid could preserve a formula so full of nutrients. Did you check microbial growth in your product? If your previous batches were ok, this problematic one could have been contamined from outside. Also, check for some signs of phase separation and pH drift (if that happened, Benzyl alcohol might have stayed in the oil phase and since you used NaOH, pH could have drifted to a more basic value, inactivating DHA and leaving your water phase vulnerable). 
  • edited October 9
    @Pharma Thank you for your insight. We are at a 5.9 pH. All the recombinant proteins, actives, and extracts were added after cooldown. I am going to do some follow-up with the lab team that batched this to triple-check everything. If we have to toss, we have to toss. 

    @ketchito PET has passed with every batch. I am going to run another round to triple check. We are currently at a 5.9 pH with this batch. These are very helpful points being made. 
  • I've used Deoplex (https://carrubba.com/deoplex-and-deoplex-organic/) with pretty decent success. It might affect viscosity , definitely test a small portion first
  • We had issue with 2%Ectoin in similar formula to yours but higher Saccharide Isomerate and Xylitol. oyster-like smell was very pronounced and browning worsen very quickly. Couldn't safe it. Hope you find the way. Best of luck.

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