What has been your most challenging formulation problem?

PerryPerry Administrator, Professional Chemist
…that you either solved or didn’t?

I had two that I recall.

First, we had this emulsion product called VO5 Cream Hairdressing that was packaged in aluminum tubes. The formula passed stability testing & was fine for a couple years of production. Then, for some reason, random batches of the product started to “bloat”. They would swell up like thick sausages and when opened, product would shoot out. It turns out there was a build-up of carbon dioxide. We never did figure out exactly what chemical reaction was taking place. Eventually, the problem just stopped happening & the investigation was stopped.

Second, some variants of our VO5 Shampoo would get cloudy - they were supposed to be clear. No problem was ever noticed in stability testing.But we found that if you cooled down some production samples they would go cloudy but would not go clear upon warming to room temperature. We figured it had something to do with the Kraft point. Adding a little glycerin seemed to solve the problem without causing too many negative effects to the rest of the formula.

ok, what are your formulation challenges you either solved or didn’t?


Comments

  • PharmaPharma Member, Pharmacist
    I'm still stuck with the idea of a stable, non-pH adjusted alcohol and propylene glycol free minoxidil solution... Using lactic acid to dissolve minoxidil in water unfortunately turns yellow quite fast. My last attempt was getting closer but still required some alcohol and diverse glycols (which still make my hair look greasy though not as bad as the standard formulation). Guess I could live with alcohol but customers more frequently demand something without it and when I'm already at puzzle solving, why not take the most challenging hike, right?
  • Hi @Pharma, on this note (sorry for a side question @Perry ), I discovered Minoxidil sulfate. Apparently it should be better than Minoxidil. What do you think about it? I'm using it at the moment, but I don't feel like it's doing much. 
  • My biggest problem until Now was to Formulate an SPF 50 Sunscreen product with just ZnO2 as a sunscreen filter... it is possible in theory but the solution is rather hard to find the way that the Distribution of the Product influences the Spf is just horror... oh and it had to be an O/W emulsion not as it would be normal due to Stability and water resistance a W/O. Still Searching for some good solutions to that problem screening the market for Raw materials for better particle distribution. 

    Head of Research and Development 
  • PharmaPharma Member, Pharmacist
    edited September 9
    @Paprik I stumbled upon this too. Never tried it.
    A few years back I couldn't find much useful but, as Wikipedia tells me (read it, it's really a helpful summary!), there is new evidence (some cool fun facts included, if you're a nerd, that is) and it also states that minoxidil sulfate (the ester, not the salt) is one of the (or the) active metabolite (weird), is highly unstable in water and ethanol (pity), is more lipophilic (weird) and still better soluble, and less likely to penetrate skin (pity). So, what you apply is most likely degraded minoxidil sulfate or just minoxidil sulfate (the salt, not the ester) and that one is probably more diluted because half the weight of it is sulfate. And I fear that aqueous solutions of minoxidil sulfate salt are as unstable as minoxidil lactate.

  • SylSyl Member
    @Pharma, it turns out that according to a dermatologist minoxidil performs better orally in low dose than as a topical solution. There was an article in the NY Times on this subject recently, the number of subjects and one picture was very convincing. The article is named An Old Medicine Grows New Hair for Pennies a Day, Doctors Say. https://www.nytimes.com/2022/08/18/health/minoxidil-hair-loss-pills.html?action=click&algo=bandit-all-surfaces-variants-time-cutoff-30&alpha=0.05&block=lone_trending_recirc&fellback=false&imp_id=985755343&impression_id=aedad4c1-1fd7-11ed-8922-95d61716deae&index=1&pgtype=Article&pool=pool%2F91fcf81c-4fb0-49ff-bd57-a24647c85ea1&region=footer&req_id=641692719&surface=eos-most-popular-story&variant=0_bandit-eng30s

  • PharmaPharma Member, Pharmacist
    @Syl That's interesting, thanks for sharing!
     Totally different approach, though :smile: (*thinks of that capsule machine sitting unused in the lab at the pharmacy*).
  • Bill_TogeBill_Toge Member, Professional Chemist
    at my last place, one of our customers wanted to expand their range with an ointment, consisting of petrolatum, mineral oil, cetearyl alcohol and cetearyl ethoxylate; as the company had ample experience with hot-fill products, the formulation itself was not difficult, but processing it was
    if you filled it too hot, it'd become rock-hard and brittle once set - you had to shear it to a smooth paste just below the melting point of the cetearyl ethoxylate and fill it below that temperature, and if the temperature got too high, the cetearyl ethoxylate would melt again and cause the end product to become granulated rather than smooth
    but once we cracked the manufacturing method, we were then able to develop a paraffin-free formula, stabilised with castor wax, which allowed more flexibility on the filling temperature (at the time there was a great deal of controversy over paraffin-based ointments starting/aggravating fires)
    UK based cosmetic chemist with 13 years' experience at the bench. I've worked with pretty much everything apart from pressed powders, soap, solid lipstick and aerosols.
  • Bill_TogeBill_Toge Member, Professional Chemist
    I also made numerous futile attempts to replicate Chinese-made styling pastes based on their ingredients lists, until I started ignoring the lists altogether and working from first principles
    UK based cosmetic chemist with 13 years' experience at the bench. I've worked with pretty much everything apart from pressed powders, soap, solid lipstick and aerosols.
  • Bill_TogeBill_Toge Member, Professional Chemist
    from my current job, the most challenging formula was a 15% azelaic acid serum - as azelaic acid is both hydrophobic and highly polar, it dissolves efficiently in very few solvents, and the ones it does dissolve in (dimethyl formamide) are highly toxic
    the solution in the end was to formulate it as an emulsion with a highly polar oil phase (butyloctyl salicylate) - it worked, and it's since become one of our best selling products
    UK based cosmetic chemist with 13 years' experience at the bench. I've worked with pretty much everything apart from pressed powders, soap, solid lipstick and aerosols.
  • PerryPerry Administrator, Professional Chemist
    @Bill_Toge - interesting challenges. I love the advice to go back and formulate from first principles. You just can’t always count on the accuracy of ingredient lists.
  • We had been producing an exfoliating wash off product for many years without any problems and would have made hundreds of tonnes in the past. 
    And then one day we started getting the odd micro issue which soon became quite frequent.
    The product was preserved with MCIT/MIT.
    The suspending agent was Aqua SF1.
    We spent ages looking at the environment and the equipment and cleaning everything up.

    No other product was affected by this contamination issue and no changes had been made to the ingredients.
    As you would imagine, when a batch was observed from start to finish there were no micro issues.

    The problem was solved by accident some time later, after I had left the company.

    The Aqua SF 1 requires (a sodium hydroxide) neutralisation step during the process.

    So instead of adding the MCIT/MIT directly to the batch (as in the instructions) some of the manufacturers were adding it into the sodium hydroxide mixture so they didn't need to walk up the stairs to add it. The sodium hydroxide solution would then be pumped in through the bottom of the vessel.
    Unfortunately the preservative was being inactivated by the dirty shortcut.




  • I am still struggling to decipher the cause of precipitation in my formulation of 4% CHG skin cleanser. The formulation has Lauramine oxide and Alkyl Polyglucoside (Caprylyl Glucoside) as surfactants and Hydroxyethyl Cellulose 100 K grade as the thickener, Glycerine as humectant, colorant, fragrance, Ethanol and 4% CHG as the active ingredient.

    Initially I thought that the APG being higher in pH is resulting in higher pH of the final product which in turn is responsible for the precipitation of CHG but the precipitation occurs even after adjusting the pH using citric acid.

    I think I need to omit the APG and formulate using only one surfactant mainly Lauramine Oxide which is somewhere neutral in nature.

    Your thoughts on this subject would be highly appreciated.
  • PerryPerry Administrator, Professional Chemist
    @MurtazaHakim - I’d suggest you try a knockout experiment.

    @Richard - compounders can certainly get creative in their methods to speed things up or make batching easier. Sometimes they work, but often it leads to problems as you’ve illustrated.
  • I am still struggling to decipher the cause of precipitation in my formulation of 4% CHG skin cleanser. The formulation has Lauramine oxide and Alkyl Polyglucoside (Caprylyl Glucoside) as surfactants and Hydroxyethyl Cellulose 100 K grade as the thickener, Glycerine as humectant, colorant, fragrance, Ethanol and 4% CHG as the active ingredient.

    Initially I thought that the APG being higher in pH is resulting in higher pH of the final product which in turn is responsible for the precipitation of CHG but the precipitation occurs even after adjusting the pH using citric acid.

    I think I need to omit the APG and formulate using only one surfactant mainly Lauramine Oxide which is somewhere neutral in nature.

    Your thoughts on this subject would be highly appreciated.

    HEC is not very compatible with glucoside
  • In an emulsion the viscosity inexplicably dropped when in contact with certain plastics, what was more weird about it was that this product was a part of a line using the same base but this only happened to that particular product and the others were totally fine. Also nothing was observed during stability , the issue only happened in contact with some plastic . the culprit was a pigment , I always thought of pigments as quite inert materials , but then this happened and still thinking about the why 

    The other formulation problem I'm obsessed with is having ascorbic acid in a water base formula that is stable (not discoloration) , so far the only way I know to have it stable is go anhydrous 
  • The project I spent the most R&D time on was duplicating the transparent Neutrogena bar soaps. For most bar soap projects being off by a percentage or two has no critical influence on final product. For this line though I can say that fractions of a percent for the key backbone ingredients affect how the bar sets and how transparent the soap crystals are (about 5 raws that all interact independently/cooperatively). Appearance and colour was also very dependent on manufacturing conditions and packaging so this project really was the ultimate case scenario for R&D at every stage in the product life.
  • FekherFekher Member, Professional Chemist
    Make hair styling product which gives shining, restylible, high fixation, no flakes, smooth effect and thanks to Allah I did it. 
  • My most challenging aspect of any formulation work is a micromanaging boss (only experience is in alcoholic beverages and ice-cream) micromanaging down to the point of 'advising' what ingredients he wants increased/decreased.

    The other big challenge I have is a marketing team changing the brief constantly. We are literally 2 weeks away from the first production run of 6 new products - all stability tests completed, micro, abrasion, fluoride stability etc - and now they want to add natural colour and other ingredients to the range - and bring in new international markets for products where we have already completed regulatory checks and formulation changes to accommodate.
  • Herbnerd said:
    My most challenging aspect of any formulation work is a micromanaging boss (only experience is in alcoholic beverages and ice-cream) micromanaging down to the point of 'advising' what ingredients he wants increased/decreased.

    The other big challenge I have is a marketing team changing the brief constantly. We are literally 2 weeks away from the first production run of 6 new products - all stability tests completed, micro, abrasion, fluoride stability etc - and now they want to add natural colour and other ingredients to the range - and bring in new international markets for products where we have already completed regulatory checks and formulation changes to accommodate.
    I love this one. Give them MBA and suddenly they know everything. Micro managing bosses, no thanks. And the ever responsive marketing team - another of my past challenges. Do what I did and don't work for anyone again and those problems go away but perhaps replaced by some others such as who is my next client.
  • Richard said:
    Herbnerd said:
    My most challenging aspect of any formulation work is a micromanaging boss (only experience is in alcoholic beverages and ice-cream) micromanaging down to the point of 'advising' what ingredients he wants increased/decreased.

    The other big challenge I have is a marketing team changing the brief constantly. We are literally 2 weeks away from the first production run of 6 new products - all stability tests completed, micro, abrasion, fluoride stability etc - and now they want to add natural colour and other ingredients to the range - and bring in new international markets for products where we have already completed regulatory checks and formulation changes to accommodate.
    I love this one. Give them MBA and suddenly they know everything. Micro managing bosses, no thanks. And the ever responsive marketing team - another of my past challenges. Do what I did and don't work for anyone again and those problems go away but perhaps replaced by some others such as who is my next client.
    That is very much the plan. I want to see the launch of these products then quit - working on the exit-plan in the background.
  • My most challenging formula was when i wanted to make a shampoo that is better than all competitors in my market. I thought the first step should be to stay away from sulfates so i started sulfate free. I tried using surfactants that on internet they were the most popular as mildest or best foam or best cleaning. I spent more than a year or even two to make such product. The problem was when i gave it and a simple with 7% SLES+ 3% CAPB to anyone for a blind test and then asked them which one did they like for not drying the skin or scalp or better cleaning or foam and they always choosed the sulfate one. And i was like what?????
    How is sulfate milder than the mildest surfactants from internet or benchmarks on internet? 
    How is sulfate cleaning better than surfactant that is theoretically claimed to have stronger cleansing power than sulfate?
    How does sulfate foam better than those surfactants that are claimed to have better or at least the same foam as sulfates?
    How no body likes sulfate free over sulfate when on internet everyone says i want sulfate free? 

    And the problem was solved when i decided to use some sulfates in any type of cleansing product no matter what or for who it is.

  • I could not thicken face wash batch containing SAlicylic, Glycolic & lactic.
    I tried more EGMS, COCOmono, HEC separate out. GUAR.
    I suspect of fragrance. & I add Lactic acid lastly.
     
     
  • I'm struggling right now in thickening the face wash. I'm trying to do a sulfate free face wash but nothing worked with me for now. I tried tylose, xanthan gum, carbopol ultrez 20, and benecel E4M.
  • PerryPerry Administrator, Professional Chemist
    @Anna_Maria what is the surfactant system?
  • Perry said:
    @Anna_Maria what is the surfactant system?
    @Perry Cocamidopropyl-betaine, glucotain clear, decyl glucoside and coco glucoside. I will try today the Sodium Cocoamphoacetate. Sodium chloride doesnt work with any of these surfactants right? 
  • @Perry also what do you think about trying PEG-150 distearate for thickening?
  • PharmaPharma Member, Pharmacist
    Sodium chloride doesnt work with any of these surfactants right? 
    Salt should work with sodium methyl cocoyl taurate, sodium cocoyl isethionate, and, most notably, sodium lauroyl methyl isethionate.
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