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Microbiology test failed twice
Hello
I have a new forumation that failed twice the microbiology test because of contamination with mesophilic bacteria .
I am using water , propanediol , polyglutamic acid (that I changed 2 so I don’t think its an issue) sodium hyaluronate , chelater and sodium anisate/sodium levulinate (same proportion used in multiple formulation that passed every test) at around 4.7pH
The only suspect is sodium hyaluronate . Did anyone ever experienced contamination on this material ?
Thx you for your time.
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31 Replies
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My guess is that your preservative system is not good. Sodium anisate/dosium levulinate is not a proper preservative. At best it is a preservative “booster”. That you passed previous challenge tests means you were lucky or your testing wasn’t suitably challenging. Almost any material can have contamination, not just sodium hyaluronate. I’d recommend putting in a proper preservative.
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Unfortunately in the french market its not possible to use phenoxiethanol or stronger preservatives. Using sodium anisate/sodium levulinate we passed 10 serums so far…except this one
Please note that we are using the hurdle approach with pH , chelator , water activity reduction .
I think that one of my materials is contaminated and wanted to know if anyone had this issue before.
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“Failed” - in challenge or manufactured QC?
That is silly system and not only likely contributor to this failure - certainly high risk for failure in consumer use whether it passed in challenge or not..
Describe your hurdle, please.
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Not failed in challenge test but failed in microbiology test (thats mandatory in EU) on account of mesophilic bacteria presence (higher than accepted norms). Our hurdle is based on Propanediol 1-3 at 3% , natural chelator (I think its evonik) at 0.15% as chelator and pH under 4.8
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Also I want to add that our shelf life is 14 months and 6 months after opening,
And the same serum passed challenge test .
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Failed twice? Two batches or did you repat the intial test?
That is not a “Hurdle” - propane diol at 3% is not effective, pH 4..8 is well within the susceptible range. Evonik - phytate? is ok.
To have a hit in QC - it’s got to be pretty bad and not comes with poor preservation but also compromised manufacturing. To address the former - can you used benzoate, benzyl alcohol what else is in your corp. policy? But please address manuf issue - have ID”d a prob cause and CAPA completed?
btw - What is technical basis for ex and PAO dating? What is your dist and shelf timing and do you really expect consumers record and to toss it at 6 months?
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Hello Phil
We did 2 separate batches . I changed the polyglutamic acid (second batch) and the only ingredient that was used on both batches is sodium hyaluronate (and propanediol , sodium phytate and preservatives)
So I am wondering if that can be contaminated.
Regarding shelf file endPAO , we do stability testing (again mandatory in EU) and chose shelf life and PAO. Its normal in France to have 6 months PAO and no benzoyl alcohol is not accepted by french customers .
Right now about 10% of the market switched to sodium anisate/sodium levulinate (natural cosmetic market) and everyone has 6 months PAO and 12-18 months shelf life.
As I said previously we passed all tests on about 10 products and a few months prior we passed another 10 using the same preservation system.
From your messages I think , that you are blaming the preservation system and not the raw materials contamination ? Did I understood correctly ?
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Hi Cdsgames,
You can do a microbiology check on the raw materials and also, you can examine a version without HA, however I doubt that HA caused the problem.
Sodium levulinate/sodium anisate - in my experience - is not a strong preservative, however, I often see products on the market using this. The reason, I guess, it might work in very simple formulations with low pH and massive amount of boosters -also with appropriate packaging- for limited time period, but in more complex systems it doesn’t do well on it’s own, I wouldn’t recommend using it alone. Also, formulations work differently from eachother - if a preservative works well in one formulation, it does not mean, it’s approppriate for another, you have to consider a lot of things when choosing the right one (incompatibilities, type of the emulsion, pH, boosters, packaging, etc.) I have to admit, I’m not an expert on this topic, but have a bit of experience. In your place I would consider changing the preservative system or using additional preservative(s) for consumer safety.
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I understand your comment - and can only offer that many use clearly inadequate preservatives systems for which levulinate/anisate is poster child EU has given the ridiculous and meaningless PAO cover - an excuse to for marketing of risky products. PAO come from the idiot EU politicians - not from industry or technology. US is not special - our politicians just passed sweeping legislation for its own sake.
I am critical of what I believe are your practices - please, not of you personally. Your development and manufacturing are not in control with poor preservation accomodated by labeling rather than formulation and inadequate control of raw material quality.
PAO - opening the product is irrelevant to preservative stability/micro safety - I know of only one preservative whose stability is reasonably impacted at opening and that is based on uses rather than time. Chemical change began to moment the product was made - a moment that might be months or years from the first use/1st opening. Even if it were significant - we KNOW consmers do not respect exp. dates, and 6 months is unrealistic if there were interested.
Good luck
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We have encountered multiple occurrences involving the utilization of Sodium Levulinate/Sodium Anisate as a preservative system. Additionally, we have been consulted by companies whose formulations incorporating Sodium Levulinate/Sodium Anisate have faced challenges in passing Production Micro testing and Quality Control.
As has been underscored, this preservative system demonstrates efficacy within controlled laboratory or ideal conditions; however, its performance is substantially contingent on the specific production processes. Some manufacturers have encountered elevated levels of Quality Control failures beyond the ordinary range.
In light of these observations, I would strongly advocate for the adoption of a more resilient preservation system.
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I just got back the new tests from lab. The raw material is not contaminated. The issue is from preservation system.
I did not disclose that we also used ferment filtrate in the serum. (that also came back negative for mesophilic bacteria). I never realized that this ferment is bug food ( info found on those forums)… So my preservation is inadequate.
I do understand that you guys advocate for stronger preservatives that will make it stable for a longer time but I do not agree with you entirely. Yes it has to be safe, absolutely, but so it’s a Mcdonald burger and yet I would rather eat a steak tartar, raw, organic if possible and preservative free. (I do not advocate for preservative free in cosmetics under any circumstance!!)
Our market is not accepting any strong preservative (sodium benzoate is grudgingly accepted)
Getting back to levulinic acid/sodium anisate, I think (I know based on all the tests) that at right ph with the right hurdles it’s a very good preservative … but far less so in emulsions. However you need to know how to use it and no the evonik mix is not good..
Anectodal problems with those preservatives do not mean much as we all understand. What ph, what ingredients, what hurdles and in what %…
I think the differences in opinions are cultural. In north America we(I grew up north) preservation means years to stays on shelfs, at least a year after opening. In the old continent, we think now, that if it stays on the shelf for more than 1 year then I don’t want to use it on my skin.
Things change and we have to change with the times.
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It is not cultural it is technical. Preservative testing is not validated to anything - neither manufacturing nor consumer ris. The asinsate/levulinate system - whatever result in challenge - clearly risks your consumers’ health, esp with the cynical 6 month PAO.
Have you ever run in-use testing?
As for manufacturing - a system that tests raw for micro contamination only after contamination is out of control in any conceot of GMP.
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Agreed. It is standard practice (or at least should be) to do a microbial check on pretty much every ingredient you use.
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Hi Phil
Can you point me to any technical data that support you statement?
Otherwise it’s just an opinion, with all due respect.
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Also you are definitely wrong on GMP, for each raw material you can accept COA (with some rules)
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Maybe read this book. This guy is pretty knowledgeable. ????
Cosmetic Microbiology: 9781138732919: Medicine & Health Science Books @ Amazon.com
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No doubt that Phil is very knowledgeable. But the big corporations have different needs in terms of shelf life and pao compared with smaller companies that don’t sell in supermarkets.
In the cosmetics market, as in real life, there are different segments. You could eat McDonald’s burgers, perfectly safe and fully validated. As for my market we would rather eat organic even thou the shelf life is less.
Meanwhile we will continue adhering to EU laws and comply with all testing procedures as mandated.
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Please don’t delegate quality/safety responsibility. Validate at least in concept a suppliers’ CDA and do not take comfort in compliance re. regulations from folks that know little to nothing of relevant technology.
The objective of preservation is consumer safety in use - not shelf life. This is not a big company fetish.
If you’d like to discuss your contamination - please provide the spec and describe OOS and process.
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I understand your point and we will certainly increase the preservation, will have to think and see what’s the best way.
In any case thx to everyone and especially Phil for sharing his vast knowledge.
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What other preservative or co-preservatives are acceptable to you besides the Sodium Anisate / Sodium Levulinate?
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The list of cosmos approved materials is short and getting shorter (pheno is out) that we can still use ..sodium benzoate is at the top of the listing .
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I am already using potasium sorbate(but less ) to augment sodium anisate
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The problem is that 2 organic acids do not have synergy ..so we are still looking at lowering further the pH and use something else to increase antimicrobial effect .
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Process and package can mitigate risk of limited preservation. Can these help in your system?
Can you use benzyl alcohol and the diols? Does your formula include a chelator?
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If you want to talk about the OOS - what were counts and ID?
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What specific Chelator are you using? You keep saying Chelator, but never define it and that makes it difficult to provide to you any really useful guidance. Are you are able to use Phenethyl Alcohol and as boosters Pentylene Glycol or 1,2 Hexanediol?
And, as @PhilGeis mentioned … what is your packaging? is the consumer able to come into direct contact with the product in the packaging such as a wide-mouth jar or even an eye dropper that is then placed back into the container? Or, are you using airless pumps? Your problem may not be just a weak preservation system, but also packaging that accentuates contamination in use.
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Sodium benzoate and Potassium sorbate have some synergy (that’s why it’s common to see then together), although it not a broad spectrum system (they are both weak against gram negative bacteria, which is your main concern in cosmetic). If you were to use only one of those, use Sodium benzoate, keeping your pH low.
All the guys that made recommendations in this post are very well known in the industry, with a lot of experience and knowledge. Their opinion is not based on habits but on solid evidence. Keep in mind that most recalled products passed all the tests you mentioned, and still failed. Those tests were all done under ideal contiditions, which are different than real life conditions. Very feq companies can afford to conduct in use micro testing, so again, please take their advice. Safety is the most important thing, and we’re responsible for that.
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I used sodium phytate as chelator. Packaging is glass bottles with dropper . I am planning to drop the pH to 4.5 and use sodium benzoate
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Why use Sodium Phytate, which raises the pH, to then have to lower the pH with a different acid? Simply use Phytic Acid as your chelator and pH adjuster.
Adding Sodium Benzoate will help because it is stronger than its analog Sodium Anisate. But, Sodium Benzoate is not really going to help you with bacterial contamination. You simply need a co-preservative that is effective against bacteria which is why I inquired if Phenethyl Alcohol was an option for you.
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Yes Phenethyl Alcohol its definitely something that we can use , do you know of sources in EU ? Do you know at what rates ?
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Need to control pH both as made and instability for benzoic - your only protection vs. fungi and staph.
Can you use benzyl alcohol?
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