iformula

By David Calvert, August 2018

We all know formulations that are complex beasts and – despite all the efforts going into turning formulation from an art to a science – it still sometimes to remain a “black-art”. Good news if you are a formulator worrying about employment prospects, but bad news if you are relatively new to the industry and are faced with either solving a problem or developing a new formulation from scratch. So what can you do?

Well, one of the tools which has been doing the rounds for a while is Design of Experiments (DoE). At its onset, it was a domain full of statistical wizardry and vulnerable to the accusation of being just smoke and mirrors. But times have moved on, not only with software advances which have made it accessible for non-statisticians, but also in terms of experience and the knowledge of how best to apply the techniques, where the pitfalls are, and how to avoid them. It has been most often used in the process and engineering sectors, but is becoming increasingly more popular in the formulation arena.

DoE can not only be used to design a formulation from scratch but also to optimise the manufacturing process – leading to a full model and that longed-for sweet spot of an optimum process. A word of caution though is that different objectives (e.g. are you aiming for screening, optimisation or robustness?) require different designs and mistakes are commonly made by choosing the wrong design or ignoring the inherent experimental errors in the measurements.

The design of a formulation is often regarded as a journey and it is so easy to get lost, even if you start with a statistical design. So how do you find the right way to develop an optimum, robust formulation and process?

Dr Paul Murray has over 20 years of implementing Design of Experiments and we are delighted that he has developed with us a new two day training course on its application to formulations. The course takes place on December 4^th and 5^th at the Jurys Inn Hotel on East Midlands airport and there is still time to book at the early bird discount rate. You can find more details of the course and how to register here.

If you would like to listen to a recording of a taster webinar, then this can also be viewed here on our website.

by Jim Bullock

It’s always good to leave the familiar bubble for a while and consider things from a different point of view. Arriving in the fascinating city of Jaipur from the UK it was striking to see TV news reports of a severe smog in Delhi. Although industrial and traffic pollution contributed to the smog, the main cause was burning of agricultural stubble on small farms. In Europe, this practice has been largely replaced by ploughing in the stubble. So this was a reminder that in the developing world, despite real advances in business and living standards, many activities that we take for granted in Europe are still restricted by the lack of access to capital resources.

The International Crop Science Conference and Exhibition (ICSCE) organised by the Pesticide Manufacturers and Formulators Association of India (PMFAI) came to Jaipur for the first time. I was struck by the high level of interest in technological advances, although the focus of these differs a little from those which we see in Europe. The Indian pesticide regulatory system sometimes makes it relatively difficult and uneconomic to develop new formulations of existing pesticides. This means that the use of in-tank adjuvants – rather than reformulation – may be a preferred technical solution to improve pesticide performance.

One similarity between India and Europe and North America is the growth in the use of biopesticides, driven by an environmental message. This is a very broad category of products which includes natural extracts and biochemical actives as well as living organisms such as bacteria and beneficial insects. Due to stability problems, biopesticides are often tricky to formulate and we should expect further advances in this area.

The industry in India seems to be in a healthy state. Several speakers mentioned that government restrictions on chemical synthesis production in China were opening up new opportunities for the economic supply of generic active ingredients from India. It will be interesting to see whether this continues.

We were delighted to be the guests of PMFAI at the event and were invited not only to present in the main conference (on developments in agrochemical formulation) but also to hold an interactive workshop. It was very gratifying to get involved in some interesting discussions and questions with participants during these sessions. Anyone who is interesting in our presentation material from these sessions should email us at info@iformulate.biz.

By David Calvert

SCS Formulate 2017 was billed as “the future of formulation” and has become a well-established event in the UK formulation calendar. The combination of a traditional exhibition (over 70 stands) with presentations from ingredients and equipment suppliers works well. At iFormulate we were pleased to be invited to present at the Inform Seminar on the subject “Cosmetic Formulators – You are Not Alone”. The explanation of the principles of systematic formulation design was well received by the attendees and if you are interested in receiving a copy of the slides, please e-mail us at info@iformulate.biz.

As would be expected, the trends at SCS Formulate were not too dissimilar from those we saw at In-Cosmetics, although the event is much more manageable in size. Anti-ageing and anti-pollution products together with natural ingredients took prime place. The six shortlisted products for the Laura Marshall Memorial Award are worth looking at in more detail if you have time.

The winner of the award was Azelis’ Maskerade which was a customisable biodegradable mask made from a cold process pectin. Interestingly the product has its origins in a cross-functional brainstorming session involving their food, pharmaceutical and personal care businesses. Of the others shortlisted, Aston Chemicals “Superfruit Splash Tint” releases water upon pressure and is claimed to also provide a mechanism for delivering aqueous actives which could be of value in other applications. Surfachem’s “Love Down Below – Intimate After Shave Balm” shows how the cosmetic industry often leads the way in breaking down social taboos!

Another area where cosmetics lead the way is in regulations which respond to consumer pressure. Emma Meredith is the Director of Science at the UK’s Cosmetic, Toiletry and Perfumery Association (CTPA) and in addition to an update on preservatives she updated attendees at the Inform session on plastic microbeads. Only recently on the BBC’s Blue Planet II, many people will have been made aware of the increasing concern around plastics in the oceans around the world. The initial target is to eliminate plastic microbeads in cosmetic and personal care products even though Emma reported that the contribution from these sources to the wider marine microplastic litter is estimated to be only 0.29%. The voluntary initiatives to remove microbeads appears to be having an effect with a CTPA survey suggesting a reduction of 70% by weight and a complete phase-out being expected by the end of 2018. Emma expressed concern over some of the definitions of plastic being proposed in some proposed UK regulations. The cited definition “a synthetic polymeric substance or any combination of polymeric substances” should cause some concern due to its breadth. Fortunately the UK seems out of step with many other countries and it is hoped that this definition with be improved before it comes into force in 2018. Personally I support the ban of “microbeads”, particularly as there are plausible alternatives in cosmetics products, but a wider scope looking at plastics, or polymers should be of concern to all formulators.

By David Calvert

Agrochemical conferences are rare in Europe and when Kisaco Research asked us to participate at their new conference in Amsterdam November 2017, then we were keen to take up the offer. As well as running a two hour workshop on “Better Formulation Design”, we presented at the main conference on “Choosing Environmentally Solvents for EC Formulations”. In addition to outlining the use of Hansen Solubility Parameters for choosing solvents, we were also able to give an overview of some of the results generated from an M.Sc project we sponsored at the University of York last year. A full paper on our findings should be available shortly and if you are interested in a copy, please let us know via info@iformulate.biz.

There is increasing pressure on synthetic pesticides from a regulatory point of view, some based on science and some not so. Where the recent furore around glyphosate fits in those extremes, I will leave to you to decide but there is no denying the increasing use of biopesticides and the further implementation of Integrated Pest Management (IPM) techniques.

One of the principles of IPM is to target application of pesticides only when and where they are needed. Technology is making great strides to assist with this trend with robots which can analyse for pests and disease and then target application. I was intrigued by one of the keynote presentations by Professor Simon Blackmore of Harper Adams University who advocated the use of small and lightweight robots which did not destroy the soil structure.

It is an interesting debate as to who is the end user of agrochemicals. If you consider the debate on glyphosate in the EU, then you may make a case that it is the general public, but conventionally it would be regarded as the farmers. The conference involved a panel session called “The Farmer’s Voice” where European Farmer’s representatives discussed the future of farming and the wishes of farmer’s for future products. Whilst welcoming new technology, they did state that the added cost of such equipment needed to be counterbalanced by a reduction in prices of the agrochemicals! There was no time to delve deeper into whether this meant overall cost (e.g. using less pesticide for the same efficacy) or simply a lower price per litre. Nevertheless, this is a challenge to formulating companies in all sectors which could lead to new business models offering not just product but full service offers. Watch this space!

By David Calvert, June 2017

It has been a strange last couple of years in global politics, and while the question “just what on Earth is going on?” may have been used in relation to Brexit, the US election, the latest UK election or Leicester City winning the English Premier League, it is still a question which as formulators we continue to ask ourselves. Whether it be changing viscosity, phase separation, product crystallising out or the product simply not working, the answer can often be found in a poorly thought out, or rushed, formulation design.

The solution to this often lies in using a formalised design process for the formulation which starts well before you actually commence your practical work. A quantified definition of what you are actually promising your customer, the competitive IP situation and essential cost and regulatory constraints are among the factors you need to consider at the onset.

Following this initial, essential preparation you commence your laboratory work where you are likely to need an experimental design approach in order to flush out the key components of your formulation, including almost certainly interactions between components. You will also need to define a preliminary manufacturing process, similarly with a definition of its key elements.

With a good laboratory programme behind you, you move to pilot stage, where you encounter scale-up issues such as mixing, heat transfer, dead-spots, cleaning and avoidance of contamination. You may have already sampled a customer with your product and could widen your product sampling at this stage.

If all progresses well, then the transfer to manufacture occurs. Ideally you will have consulted with your manufacturing colleagues well before this stage, rather than this being the first time they have heard they need a novel mixer, or a large scale “spatula”. Here you will understand what are the critical elements of the process are and what control strategies you envisage.

With successful manufacture, you then reap the benefits of all the hard work and can use the knowledge gained to go forward and develop your next range of products.

Risk assessments form an essential element of the “stage-gate” type approach to development that you will need to take. As you move through the process and the risks should be better defined and reduced, the closer you get to production and commercialisation.

We call this systematic approach “Design for Formulation” and if you want to learn more, we are running a two day training workshop at Jury’s Inn Hotel, East Midlands Airport, in the UK on September 19^th and 20^th. You will hear from experienced practitioners such as our Associate Partner Ian Jolliffe, David Hood from the Excellence Partnership, Phil Threlfall-Holmes of TH Collaborative Innovation (THCi) and Olivier Cloarec of Sartorius-Stedim.

There are two webinars available where you can hear David and Ian talk about different elements of the process. Follow the links below – and send an e-mail to info@iformulate.biz if you require passwords.

– iFormulate introduces…Ian Jolliffe on “Design for Formulation”

– iFormulate introduces…Process Control and Formulation

Details about the course and how to register before the August 1^st early bird deadline can be found on the event web page.

By Jim Bullock, April 2017

Small can be beautiful of course but sometimes events can improve while they grow in size. The fourth “Spray Drying and Atomisation of Formulations” course, hosted by the University of Leeds, is a case in point. Starting in 2014 with around twenty delegates and two days of content, the course is now three days in length with over twenty presentations, six laboratory demonstrations, seventeen lecturers (from industry and academia), sixty delegates and one ever-popular course dinner. Each year I am impressed by how many new applications for spray drying are discussed, either in the formal sessions or during the informal opportunities to talk.

In 2017, delegates came from all parts of Europe and some from further afield. There was a big contingent from the pharmaceutical industry (where spray drying is really gaining a foothold for a number of uses) as well as from food & drink (think infant formula milk), speciality chemicals, agrochemicals, detergents and ceramics.

Although the science of spray drying is well understood, during the panel sessions, the expert lecturers were of the opinion that progress can still be made in predictive modelling and in-process analytics. Challenges still remain in energy recovery and (for pharmaceuticals) to make the technique a more universal alternative to freeze drying.

As ever, thanks should go to the energetic organisational support from the CPD team at the University of Leeds Faculty of Engineering who have had to deal with an increasingly complex course over the years. The 2017 course was sold out, so to make sure you don’t miss out in 2018, have a look at the course web-page and then – to express an interest in attending – please email cpd@engineering.leeds.ac.uk.