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Physico-Chemical Properties of Poloxamer Surfactants Related to Their Adsorption

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Physico-Chemical Properties of Poloxamer Surfactants Related to Their Adsorption Physico-chemical properties of poloxamer surfactants related to their adsorption. Submitted March 1996 The School of Pharmacy University of London David Leonard Carthew ProQuest Number: 10104236 All rights reserved INFORMATION TO ALL USERS The quality of this reproduction is dependent upon the quality of the copy submitted. In the unlikely event that the author did not send a complete manuscript and there are missing pages, these will be noted. Also, if material had to be removed, a note will indicate the deletion. uest. ProQuest 10104236 Published by ProQuest LLC(2016). Copyright of the Dissertation is held by the Author. All rights reserved. This work is protected against unauthorized copying under Title 17, United States Code. Microform Edition © ProQuest LLC. ProQuest LLC 789 East Eisenhower Parkway P.O. Box 1346 Ann Arbor, Ml 48106-1346 for Amanda, Acknowledgements I would like to thank my supervisor Dr. Graham Buckton for his help and assistance throughout this PhD and for his acceptance of my odd working hours! The Wellcome Foundation for their financial support, and the assistance of Steve Poole and Dr. Gary Parsons with the development of the project. All the technical staff at the School of Pharmacy for their support setting up experiments, especially Brian Bissenden for his help with the Hydrophobic Interaction Chromatography, and his sporting comments! My fellow PhD students throughout the three years. Particular mention must go to Suki Mall for being a friend throughout, and for her wonderful dinner parties. I would also like to thank my friends and family, special thanks must go to mum for proof reading the thesis. Abstract 4 The properties of poloxamer surfactants were investigated by a number of techniques. The adsorption of PI 88, P338 and P407, was studied on range of solids. The solids used were hydrophobic and poorly water soluble. An effect of temperature on the adsorption behaviour of the three surfactants was noticed. Poloxamers undergo a transition at a temperature which is dependent on their poly(oxypropylene) content, resulting in the amount of poloxamer adsorbing increasing. The transition can be attributed to a dehydration of the poly(oxypropylene) core of the poloxamer molecule, corresponding to changes in the micellar behaviour of the surfactants. The CMC is highly dependent on temperature. The nature of the adsorbate was found to affect poloxamer adsorption. The surface nature of the solids was investigated using contact angles. The poloxamers were investigated for their surface energy using different methods, and considered as both complete molecules and the sum of their individual components. Poloxamers do not adsorb readily to solids which have higher surface energies or which are more polar, suggesting that knowledge of surface nature could be useful in predicting adsorption behaviour. A model surface was created using chlorotrimethylsilane coated glass. It was possible to produce an artificial surface with known repeatable surface energy. Poloxamers adsorb to the coated slides. Slides with poloxamer adsorbed were shown to have altered surface nature. The hydrophobicity of the plates decreased as poloxamer adsorbed. Abstract 5 The effect of temperature on the poly(oxyethylene) component of the poloxamer molecule was investigated by two techniques. Hydrophobic Interaction Chromatography and Photon Correlation Spectroscopy. It was shown that the poly(oxyethylene) reduced in size with increasing temperature. The hydrophobicity does not alter significantly with changes in temperature. These two techniques were also shown to substantiate the effects of temperature on the poly(oxypropylene) shown through adsorption studies. Aims and Objectives 6 It was decided to investigate the properties of poloxamer surfactants in greater detail than had been done previously. The effects of temperature on adsorption of poloxamers and the effect of altering the temperature after adsorption had taken place. The actual method of poloxamer adsorption and to some extent its behaviour in other situations. It was also a priority to see if knowledge of poloxamer surface energy and solid surface energy could be used as either values or rules, in an ‘expert system’ for predicting and optimising poloxamer use in liquid systems such as suspensions and emulsions. Table of Contents 1 Acknowledgements...................................................................................... 3 A b stract...........................................................................................................4 Aims and objectives .....................................................................................6 Table of contents .......................................................................................... 7 List of Tables................................................................................................19 List of figures................................................................................................24 List of symbols ............................................................................................29 1 Introduction ...............................................................................................................32 1.1 Surfactants....................................................................................................................32 1.1.2 Types of surfactant ...................................................................................................... 34 1.1.3 Micelles and other surfactant structures ...................................................................34 1.1.4 Uses of surfactants .......................................................................................................36 1.2 Poloxam ers................................................................................................................. 36 1.2.1 Introduction to poloxamers ........................................................................................ 36 1.2.2 Other similar block co-polymers ............................................................................... 37 1.2.3 Nomenclature of poloxamers .....................................................................................38 1.2.4 Uses of Poloxamers ..................................................................................................... 39 1.2.5 Using poloxamers for targeting ................................................................................. 40 1.2.6 Other uses for poloxamers ..........................................................................................41 1.2.7 Properties of poloxamers ............................................................................................42 1.2.7.1 Micellation ................................................................................................................ 42 Table o f Contents 8 .2.7.2 Effect of temperature on micellation .....................................................................44 .2.8 Transition temperatures in poloxamers .................................................................... 46 .2.9 Poloxamers forming gels ............................................................................................ 47 .2.10 Poloxamer adsorption ............................................................................................... 47 .3 Surface Energy.............................................................................................................. 49 .3.1 Introduction to surface energy ................................................................................... 49 .3.1.1 Surface Parameters...................................................................................................49 .3.1.2 Solid / Liquid interactions ....................................................................................... 50 .3.1.3 Wetting .......................................................................................................................51 .3.2.1 Surface tension measurement ................................................................................. 53 .3.2.2 The Wilhelmy plate technique for surface tension measurement ......................53 .3.3.1 Contact angle measurement .................................................................................... 55 .3.3.2 Liquid penetration .................................................................................................... 55 .3.3.3 Methods of contact angle analysis using powder compacts ............................... 56 .3.3.4 Hysteresis in contact angle measurement ..............................................................56 .3.3.5 The Wilhelmy plate ..................................................................................................58 .3.4 The use of contact angles to determine surface energies ....................................... 59 .3.4.1 Critical surface tension ............................................................................................ 59 .3.4.2 The Good & Grifalco interaction parameter .........................................................59 .3.4.3 The geometric and harmonic mean equations ......................................................60 .3.4.4 Calculation of polar and dispersive components of surface tension ................. 63 .3.4.5 Neumann’s equation of state .................................................................................. 63 .3.4.6 Wu’s equation of state ............................................................................................
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