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Study on In-process Liquid Crystalline Capsules for Cosmetic Applications : Fabrication, Characterization, Evaluation and Clinical Trials
- 주제(키워드) in-process lipid crystalline (IPLC) capsule , fatty amphiphile , polymorphic lattice , encapsulation
- 발행기관 아주대학교
- 지도교수 박영준
- 발행년도 2019
- 학위수여년월 2019. 8
- 학위명 박사
- 학과 및 전공 일반대학원 응용생명공학과
- 실제URI http://www.dcollection.net/handler/ajou/000000029093
- 본문언어 영어
- 저작권 아주대학교 논문은 저작권에 의해 보호받습니다.
초록/요약
Many kinds of lipid capsules have been applied for cosmetics since capsules could provide visual attractiveness and encapsulate the functional actives. However, most of these lipid capsules are fabricated in the separate off-line process and post-added onto cosmetic manufacturing process causing the more complexity. Moreover, these lipid capsules used to utilize the synthetic colorants or potentially uncertain inorganic components to expose the capsule images and to enhance the compatibility in cosmetic chassis. In-process lipid crystalline (IPLC) capsules for which internal phase was comprised of in-processed lipid particles simultaneously formed onto emulsion manufacturing process and external phase remained transparent exposing the lipid capsules more outstandingly was fabricated slightly modifying liquid crystalline lamellar gel network-forming emulsion process by applying high molecular weight fatty alcohols only. The capsules exhibited wide range of macroscopically visible lipid particles dependent on lipid ratio and agitating & homogenizing processing conditions and represented mean particle sizes of 350~450 μm for the majority, displaying 50~2,000 μm in size distribution which was most attractive in appearance for skin cosmetic application. The lipid capsules appeared to be best formed in the conditions with 10 : 1 ratio of behenyl alcohol and batyl alcohol and with low energy processing inputs for manufacturing. These lipid capsules fabricated in this method presented round and soft cushiony characteristics with 45 % capsule phase occupied in emulsion, demonstrating smooth spreadability with velvety feel when rubbed and displaying refractive birefringent crystalline views under a polarized microscopy. Several rheological tests were performed to assess the storage stability, spreadability and applicability considering skin application. In these series of tests IPLC capsules represented the non-Newtonian, pseudo-plastic, shear-thinning, thixotropic and solid-like elastic behavior characteristics for which yield point was in the range of 50 pa, demonstrating its good potentials in both visual appearances and sensory feels for skin. And in the continued temperature-dependent oscillation test, IPLC capsules exhibited two temperature-related phase phenomena at 45 ℃ and 67 ℃ which were higher than normal room temperature, implicating that IPLC capsules would be sufficiently robust against potential room temperature change for long-term storage condition. And its Tan δ which could measure the degree of viscoelasticity appeared to be 0.14 for which IPLC capsules would be structured with elastic properties rather than viscous one, indicating good applicability for skin. The long-term aged stability test on IPLC capsules also revealed to be stable over 6 months under 5 ℃ / 25 ℃ / 40 ℃ without phase separation or blurring of transparency. And the experiments on lipid crystalline capsule structure using DSC revealed that endothermic peaks of IPLC capsules showed the higher melting phenomena than individual fatty lipid component and also demonstrated high encapsulating potentials for which the crystallinity index reached to more than 42 %. And the SAXS and WAXS techniques revealed that IPLC capsules consisted of Lß’-crystalline orthorhombic phase in polymorphic lattice displaying two peaks with short d-spacing 0.41 and 0.37 nm, and inter-layer long d-spacing between hydrophilic and hydrophobic region was constituted with 6.5 nm in distance. It was figured out that it was slightly swollen over 10% by electrostatic repulsion and hydrophobic attraction forces of both fatty alcohol amphiphiles in water system, considering that behenyl alcohol and batyl alcohol mixture only displayed 5.9 nm in distance and carbon chain length (C-C bond length) per one unit was considered to be 0.025 nm. To confirm encapsulation performances of IPLC capsules, both ATI (lipophilic vitamin C derivative) and borage oil containing 20 % GLA were formulated, stimulating them to incorporate into lipid crystalline lattice. And it was revealed that more than 75 % for ATI and 95 % for GLA were incorporated into in-process crystalline lipid polymorphic lattice. And in the occlusion test it also demonstrated 35.1 % better performance versus membrane only (control I) and also 16.9 % better versus non-capsule emulsion (control II) in the capability of suppressing the water vapor evaporation when the PES-type artificial membrane was applied. And in Franz cell test to confirm delivery capability of active components, IPLC capsules represented 1.4 ~ 3.4 folds of higher release and penetration performances across the tested period, indicating that micronized lipid crystalline particles in lamellar gel phase rubbed on skin would form the artificial barrier layer, promoting GLA released and penetrated more quickly and deeply (Figure 2-6). In 4 weeks clinical trials to 21 skincare expert panels, IPLC capsules represented excellent skin whitening & skin firmness improvement within statistically 95 % significance level - 0.41 % for whitening and 5 % for firmness better - for each. And it was also confirmed that the degree of satisfaction after 4 weeks use was surveyed for 86.4 % which could be regarded significantly higher than each respective questionnaire. Last but not least, IPLC capsules did not show any irritation potentials to skin in the clinical trial, proving that it was formulated with fail-safe components.
more목차
CHAPTER I Fabrication & Characterization of IPLC Capsules ----------------------------1
1-1. Introduction & Objective ---------------------------------------------------------------- 1
1-1-1 Introduction ------------------------------------------------------------------------------1
1-1-2 Objective ---------------------------------------------------------------------------------4
1-2. Materials and Methods -------------------------------------------------------------------5
1-2-1 Materials ----------------------------------------------------------------------------------6
1-2-2 Preparation of IPLC Capsules ----------------------------------------------------------7
1-2-3 Microscopy, Morphology, Particle Size --------------------------------------------10
1-2-4 Degree of Capsule Formation---------------------------------------------------------10
1-2-5 Rheological Characterization on IPLC Capsules -----------------------------------11
1-2-6 Stability -----------------------------------------------------------------------------------11
1-3 Results & Discussion -----------------------------------------------------------------------12
1-4 Conclusion ----------------------------------------------------------------------------------26
1-5 References ----------------------------------------------------------------------------------28
CHAPTER II Fabrication & Characterization Containing Skin Functional Actives ---31
2-1 Introduction & Objective ----------------------------------------------------------------31
2-1-1 Introduction ----------------------------------------------------------------------------31
2-1-2 Objective --------------------------------------------------------------------------------32
2-2 Materials and Methods ------------------------------------------------------------------33
2-2-1 Materials ---------------------------------------------------------------------------------33
2-2-2 Partitioning Coefficient and Polarity of ATI and GLA ---------------------------35
2-2-3 Differential Scanning Calorimeter, Crystallinity Index ----------------------------35
2-2-4 Small-and Wide-Angle X-ray Scattering Measurement (S/WAXS) ------------36
2-2-5 Analysis on Encapsulation Efficiency by HPLC and GC --------------------------36
2-3 Results & Discussion ----------------------------------------------------------------------37
2-4 Conclusion ---------------------------------------------------------------------------------49
2-5 References ---------------------------------------------------------------------------------51
CHAPTER III In-vitro Evaluation & Clinical Trials of IPLC Capsules for Skin ----------54
3-1 Introduction & Objective ----------------------------------------------------------------54
3-1-1 Introduction ----------------------------------------------------------------------------54
3-1-2 Objective --------------------------------------------------------------------------------56
3-2 Materials and Methods -------------------------------------------------------------------57
3-2-1 Materials ---------------------------------------------------------------------------------57
3-2-2 Occlusion Test (Inhibition of Water Vapor Transmission Rate) ----------------57
3-2-3 In-vitro Trans-epidermal Release & Penetration Study by Franz Cell --------57
3-2-4 Skin Firmness Evaluation using Visia CR ------------------------------------------71
3-2-5 Skin Whitening Evaluation using Chromameter --------------------------------71
3-2-6 Technical Qualitative Survey on IPLC Capsules for Skin------------------------71
3-3 Results & Discussion ---------------------------------------------------------------------58
3-4 Conclusion ---------------------------------------------------------------------------------64
3-5 References ---------------------------------------------------------------------------------67
