iPRD : Case Studies

Dr James Tunstall

Outline

1) Introduction

2) Case Study 1 : Selenol Project

3) Case Study 2 : DeltaG Nutraceutical

4) Case Study 3 : Joomo

5) Case Study 4 : Coffee Metabolites

6) Case Study 5 : Polymeric drug delivery system

iPRD : innovative Process Research and Development

Specialise in all aspects of process development ranging from:

1. Route design

2. Reaction scaling

3. Process engineering

4. Formulation

Introduction

Selenol Project

Background

Selenol and diselenides have a wide application in high end electronics and are known to be used in photovoltaic cells found in solar panels.

Synthesis of Selenols on scale can be problematic with associated odours, toxicity and the tendency of Selenols to undergo rapid oxidative dimerisation in the presence of O2.

Original Process

Number of problems : Poor Yield (40 – 50 %) and subsequent selenium waste. Highly Toxic H2Se byproduct

Case Study 1

Case Study 1

New Process

1. The new process produces almost quantitative yield of the desired selenol.

2. Removes the formation of the toxic malodourous H2Se.

3. Intermediate deselenide is a distillable stable liquid; allowing storage.

TΔS – Nutraceutical

Background

Product is a high value nutraceutical in human trials based on the science of ketone-bodies in human nutrition. Ketone-bodies have a key role in nutrition as highly efficient 'brain and muscle food'. TΔS have identified proprietary precursors that, for the first time, enable the amounts of ketones in our bodies to be elevated, bringing a range of benefits.

Current Process

The original batch process was catalysed by a heterogeneous catalyst for 5 days.

Issues :

1. Extended reaction times produced various impurities2. Scale up with current catalyst loading was prohibitively expensive

Case Study 2

.

Case Study 2

300mm

300mm

300mm

Pressure Gauge Port

Plug Flow Reactor

Plug Flow Reactor

Moving to a continuous system :

1. Reduced reactions times from 5 days to 1 h

2. Shorter reaction times produced fewer impurities

3. Reduced catalyst loading required for 50 kg batch - from 12 kg to 100 g of catalyst.

Overall this produced significant cost savings by making the process much more efficient.

Case Study 2

http://www.tdeltas.com/index.htm

Case Study 3

JOOMO : Natural face cream

Background

Start-up company with an new skincare product required large batch for further trials but no in-house capabilities

Original process

Initial product formulation led to variance in product homogeneity caused by frothing.

http://www.joomo.coop/

Original formulation

Case Study 3

After two week exploratory work to ensure successful manufacture we delivered two 20 kg batches on time and to customer specifications

This enabled distribution of free product samples during the Christmas shopping period.

New formulation

Case Study 4

Coffee Metabolites Study

Background

We were asked to synthesise a variety of coffee metabolites recently identified in human plasma and urine after consumption of coffee.

Summary

We produced multigram quantities of these metabolites for use as analytical standards in a food science study.

*Barron, D, et al.; Org. Biomol. Chem., 2010, 8, 5199–5211

Case Study 5

Polymeric drug delivery

Background

We were contracted to synthesise a variety of polymeric backbones for use as novel drug delivery systems. These particular systems have been successful in delivering various drug payloads including chemotherapy treatments.

Summary

We have successfully scaled the polymer synthesis to produce multigrams of the desired polymer backbone. We are in the process of grafting a fluorescence stains to allow visual monitoring of the polymer during ex vivo studies.

Chen, R.; Eccleston, M.; Yuec, Z.; Slater, N.;*, J. Mater. Chem., 2009, 19, 4217–4224

Summary

We have a broad skill base ranging from chemical synthesis to process design and engineering. Our facilities allows to produce materials ranging from grams for use as analytical samples up to kilos of material for more extensive testing.

Acknowledgements

Prof. John BlackerProf. Philip Kocienski

Prof. Frans MullerDr. John Cooksey

Susan PollardJanet Welch