A primary emulsion with whey protein isolate (WPI) and hexanoic acid was prepared, and chitosan (Ch) (0.01%, 0.02%, and 0.03%) was added to evaluate its impact on particle size distribution of the emulsion. NaCl (0, 20, 40, and 80 mM) was added to increase ionic interactions to stabilize the multilayer emulsion. Lecithin (0.5%, 1%, 2%, 3 %, w/v) was mixed with the primary emulsion in order to form a multilayer, and casein hydrolysate (CH) was used to stabilize the tertiary emulsion system without the use of NaCl for 28 d at 4 °C. Stable O/W nanoemulsions were generated for use as nano-vesicular vehicles (NVV) to carry Curcumin (CU). Two important variables, (1) addition of casein hydrolysate (CH) (1:50, w/w WPI) and, (2) use of high pressure (140 and 210 MPa), were studied for their effect on the stabilization of monodispersed NVV and persistence of antioxidant activity of the CU as cargo in the NVV throughout storage. Addition of CH reduced nano-particle size and increased emulsion stability with UHPH pressure. The nanoparticle distribution was not changed by the addition of CU. Addition of casein hydrolysate reduced particle size as well as enhanced the positive functional properties of the NVV. Similar trends were observed in zeta-potential, surface energy, contact angle and antioxidant efficacy of the NVV, both with and without CU when UHPH was applied. The effect of Ultraviolet (UV) radiation (254 nm) on the stability of O/W nanoemulsion systems was investigated. A nano vesicular vehicle (NVV) was generated using ultra-high pressure homogenization (UHPH) that was stabilized using whey protein isolate (WPI) (1%, w/v), Tween 20 (20% w/w WPI) and casein hydrolysate (CH) (1:50 of WPI, w/w). Coarse emulsions were prepared by blending for three min. The coarse emulsion was exposed to UV radiation (0-60 min), followed by a single-pass of UHPH at 140 and 210 MPa. The UHPH treated NVV-CU had greater (P<0.05) short and long term antioxidant properties. After 28 d of storage, the CU-NVV treated at 210 MPa retained 7.0 and 1.4% greater AA and AP, respectively, when compared to the unpressurized CU-NVV.

京都大学 / 新制・課程博士 / 博士(農学) / 甲第23248号 / 農博第2455号 / 新制||農||1084(附属図書館) / 学位論文||R3||N5338(農学部図書室) / 京都大学大学院農学研究科農学専攻 / (主査)教授 松村 康生, 教授 丸山 伸之, 教授 谷 史人 / 学位規則第4条第1項該当 / Doctor of Agricultural Science / Kyoto University / DGAM

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High Pressure Liquid Chromatography (HPLC) is a well-known and widely used analytical technique which is prevalent throughout the pharmaceutical industry as a research tool. Despite its prominence HPLC possesses some disadvantages, most notably slow analysis time and large consumption of organic solvents. Ultra Pressure Liquid Chromatography (UPLC) is a relatively new technique which offers the same separation capabilities of HPLC with the added benefits of reduced run time and lower solvent consumption. One of the key developments which facilitate the new UPLC technology is sub 2-µm particles used as column packing material. These particles allow for higher operating pressures and increased flow rates while still providing strong separation. Although UPLC technology has been available since early 2000, few laboratories have embraced the new technology as an alternative to HPLC. Besides the resistance to investing in new capital, another major roadblock is converting existing HPLC methodology to UPLC without disruption. This research provides a framework for converting existing HPLC methods to UPLC. An existing HPLC method for analysis of Galantamine hydrobromide was converted to UPLC and validated according to ICH guidelines. A series of statistical evaluations on the validation data were performed to prove the equivalency between the original HPLC and the new UPLC method. This research presents this novel statistical strategy which can be applied to any two methodologies to determine parity. / Chemistry

This thesis consists of a thermodynamically based kinetic model that more accurately predicts grain boundary mobility (GBM) over a large range of thermodynamic states including changes in temperature, pressure and shear stress. The form of the model was validated against calculated GBM values for Al bicrystals via molecular dynamics (MD) simulations. A total of 98,786 simulations were performed (164 different GBs, each with a minimum of 250 different thermodynamic states, and 2 different driving forces). Methodology for the computation of the GBM via MD simulations is provided. The model parameters are directly linked to extensive thermodynamic quantities and suggest potential mechanisms for GBM under combined thermal and triaxial loads. This thesis also discusses the influence of GB character on the thermodynamic mobility parameters. The resulting insights about GB character and thermodynamic state on GBM suggest an opportunity to achieve designed microstructures by controlling thermodynamic state during microstructure evolution.

Résumé : L'interaction entre la β-Lactoglobuline (β-Lg) et le rétinol ou entre les micelles de phosphocaséines (PC) et le rétinol à un pH proche de la neutralité, a été étudiée à pression atmosphérique et sous pression isostatique jusqu'à 400 MPa. Les constantes de dissociation et le nombre de sites de liaison ont été calculés indiquant des différences d'affinité en fonction de la structure protéique. A 25°C, des pressions inférieures à 150 MPa favorisent l'association β-Lgrétinol (rapport molaire β-Lg/rétinol : 1/1). A ≥ 150 MPa le complexe se dissocie. A 350 MPa, la β-Lg est dénaturée et le complexe irréversiblement dissocié. Le complexe PCrétinol (rapport molaire PC/rétinol : 1/1) reste au contraire formé après un traitement à 400 MPa et 25°C, bien que la pression induise des phénomènes de dissociation/réassociation des assemblages micellaires à ≥ 100 MPa. L'interaction PCrétinol stabiliserait plutôt les micelles de PC vis-à-vis de la pression, de même qu'une température de pressurisation modérée (35°C) comparativement à une température plus basse (15°C). Un isolat protéique de lactosérum (IPL) en dispersion dans l'eau à 10% (p/p) de protéines (pH 6,5) et en présence d'acétate de rétinol (AcRet) (rapport molaire β-Lg/AcRet : 10/1) a été traité par (i) haute-pression isostatique (HP) (350 MPa, 25°C, 15 min), (ii) traitement thermique de courte durée (TTCD) (75°C, 4 s) ou (iii) homogénéisation à ultra-haute pression (UHPH) (300 MPa, Tin = 24°C). Les trois traitements permettent de former des agrégats de β-Lg capables de retenir l'acétate de rétinol, mais avec une efficacité différente dépendant probablement des mécanismes d'agrégation induit par le chauffage (TTCD), la pression isostatique (HP) ou dynamique (UHPH). Des dispersions à 2,38% (p/p) en phosphocaséines (pH 6,6) en présence d'acétate de rétinol (rapport molaire PC/AcRet : 5/1) ont été traitées par (i) HP (300 MPa, 14°C ou 34°C, 15 min), ou (ii) UHPH (300 MPa, Tin = 14°C). Ces deux traitements favorisent la rétention de l'acétate de rétinol par les micelles de PC pouvant ainsi servir de cargo pour véhiculer des molécules bioactives. Mots clefs : haute pression isostatique, haute pression dynamique, homogénéisation à ultra-haute pression, fluorescence, β-Lactoglobuline, micelles de phosphocaséines, rétinol, acétate de rétinol, agrégats protéiques, interaction protéine-ligand. / Abstract: The binding of retinol to native β-Lactoglobulin (β-Lg) or phosphocasein (PC) micelles at pH close to neutral was studied at atmospheric pressure or under isostatic high-pressure. The dissociation constants and number of binding sites were calculated indicating that difference in retinol affinity depended on protein structure. At 25°C, pressure level < 150 MPa promoted β-Lgretinol association (β-Lg/retinol molar ratio: 1/1). At ≥ 150 MPa, the complex dissociated. At 350 MPa, β-Lg was denatured and the complex irreversibly dissociated. PC and retinol (PC/retinol molar ratio: 1/1) remained associated after pressurisation at 400 MPa and 25°C, while pressure induced dissociation/reassociation phenomena of micelle assemblies. The binding of retinol to PC stabilised micelles towards pressure, as well as moderate temperature of pressurisation (35°C) compared to lower temperature (15°C).A whey protein isolate (WPI) dispersed in water at 10% (w/w) proteins (pH 6.5) in the presence of retinyl acetate (RetAc) (β-Lg/RetAc molar ratio: 10/1) was processed by (i) isostatic high-pressure (HP) (350 MPa, 25°C, 15 min), (ii) short-time thermal treatment (STTT) (75°C, 4 s) or (iii) ultra-high pressure homogenisation (UHPH) (300 MPa, Tin = 24°C). All processing produced β-Lg aggregates able to retain RetAc, but with different efficiency depending on aggregation mechanisms induced by heating (STTT), isostatic high-pressure (HP) or dynamic high-pressure (UHPH). Phosphocaseins dispersed at 2.38% (w/w) proteins (pH 6.6) in the presence of RetAc (PC/RetAc molar ratio: 5/1) were processed by (i) HP (300 MPa, 14°C or 34°C, 15 min), or (ii) UHPH (300 MPa, Tin = 14°C). Both treatments promoted RetAc retention by phosphocasein micelles that can be used as cargoes to transport bioactive molecules.Keywords: isostatic high-pressure, dynamic high-pressure, ultra-high pressure homogenisation, fluorescence, β-Lactoglobulin, phosphocasein micelles, retinol, retinyl acetate, protein aggregates, protein-ligand binding.Discipline: Biochimie, Chimie et Technologie des Aliments.Thèse préparée à : Université Montpellier 2 – Equipe de Biochimie et Technologie Alimentaire – UMR IATE 1208 – Pôle EVAP – Place E. Bataillon, 34095 Montpellier, France.

This master thesis covers the development of a high-pressure fuel system for compression ignitedfuels such as diesel and diesel-like fuels that will be deployed into a single cylinder test cell at AVLMTC Södertälje, Sweden. The test cell is used by AVL to conduct research and testing of new fuelsfor their customers and this new fuel system will widen the span of fuels able to be tested by theequipment.This thesis focuses on pumping and pressurizing of the fuel, ensuring that all ingoing materialsare non-corrosive in this environment and compatible with the necessary fuels and lastly a safetyanalysis of the system with respect to operator and process safety. Other aspects of the projectsuch as mass flow measurements and fuel conditioning is covered in a sister thesis Mass flowrate measurement of compression ignition fuels in high-pressure stand-alone pump unit for singlecylinder test cell written by C. Aksoy [1].The goal of this thesis project was to deliver a finished manufactured fuel system and if the timeallowed for it, also validate its performance and finally installing and incorporating it into the singlecylinder test cell. The development process started with the writing of a product specificationoutlining the requirements and request on the product in a specification of requirements matrix andrelate these to product properties of the system using a quality function deployment (QFD) matrix.This document was then used as a base for further advancement in developing concepts to solveeach product property and weighing these concepts against each other using Pugh’s matrices. Thechosen concepts were then further developed, a flow chart for the system was developed as well asfuel lines and other supporting components were analyzed and chosen.In the end the high-pressure fuel pump from Scania’s XPI fuel system were chosen as well asa pressure transducer in the HP1000 series from ESI. Within the time frame of this thesis, theproject did not end up getting finished to the degree planned, but due to time constraints werehalted before starting manufacturing of the system. Some minor component choices remained aswell as documentation such as drawings and finalizing the physical layout of the system remained.All information regarding the remaining work needed to finalize the project and deploying thesystem in the test cell were outlined and with more time, the fuel system should fulfill its purposeof allowing testing and research of compression ignited fuel to be possible in the test cell. / Kontentan för denna mastersavhandling är utvecklingsprocessen för ett högtrycksbränslesystemför kompressionsbränslen såsom diesel och diesellika bränslen som kommer att installeras i enencylindertestcell hos AVL MTC Södertälje, Sverige. Testcellen används av AVL för forskningoch testning av nya bränslen åt deras kunder och detta nya bränslesystem kommer att utöka typernaav bränslen som kan testas med utrustningen till att inkludera kompressionsantända bränslen.Denna avhandling fokuserar på utvecklingen av tillförseln och trycksättnigen av bränslet, säkerställnigenav att ingående material är icke-korrosiva i den avsedda miljön och kompatibla med allanödvändiga bränsletyper och slutligen en säkerhetsanalys av systemet med avseende på operatörsochprocessäkerhet. Andra aspekter såsom massflödesmätning och bränslekonditionering presenterasi systeravhandlingen Flödesmätning och konditionering av högtryckantända bränslen för encylindertestcellskriven av C. Aksoy [1].Målet med denna avhandling var att leverera ett färdigtillverkad bränslesystem och om tiden tillät,även validera systemets prestanda och slutligen integrera och installera systemet i testcellen. Utvecklingsprocesseninleddes med att skriva en produktspecifikation som innehöll en sammanställningav kundens krav och önskemål för produkten och relaterade dessa till produktegenskaper med hjälpav en quality function deployment (QFD) matris. Detta dokument användes vidare som en bas förfortsatt utveckling av produkten i konceptgenereringsprocessen och för att väga de olika konceptenmot varandra med hjälp av Pugh’s matriser. De valda koncepten blev sedan analyserade ytterligare,ett flödesschema för de ingående komponenterna framtaget och övriga sekundära komponenteranalyserade och valda.Till slut valdes högtrycksbränslepumpen från Scanias XPI system och en tryckgivare från HP1000-serien från ESI. Inom tidsramen för avhandlingen färdigställdes aldrig projektet till den grad somhade planerats, men blev istället avbrutet innan tillverkningen av systemet han påbörjas på grund avtidsbegränsningar. Vissa sekundära komponentval, dokumentation såsom ritningar och färdigställningav den fysiska layouten av systemet kvarstod vid avhandlingens slut. All information angåendeallt nödvändigt fortsatt arbete för att färdigställa projektet och integrera systemet i encylindertestcellendokumenterades och med mer tid borde bränslesystemet kunna uppfylla sitt syfte att möjliggöratestning och forskning av kompressionsbränslen i testcellen.