Spruce Bark Extract As a Sun Protection Agent in Sunscreens
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Mengmeng Sui Spruce bark extract as a Sun protection agent in sunscreens School of Chemical Engineering Master’s Program in Chemical, Biochemical and Materials Engineering Major in Chemical Engineering Master’s thesis for the degree of Master of Science in Technology Submitted for inspection, Espoo 21.07.2018 Thesis supervisor: Prof. Tapani Vuorinen Thesis advisors: M.Sc. (Tech.) Jinze Dou Ph.D. Kavindra Kesari AALTO UNIVERSITY SCHOLLO OF CHEMICAL ENGINEERING ABSTRACT Author: Mengmeng Sui Title: Spruce bark extract as a sun protection agent in sunscreens Date: 21.07. 2018 Language: English Number of pages: 48+7 Master’s programme in Chemical, Biochemical and Materials Engineering Major: Chemical and Process Engineering Supervisor: Prof: Tapani Vuorinen Advisors: M.Sc. (Tech.) Jinze Dou, Ph.D. Kavindra Kesari This study aimed to clarify the feasibility of utilizing spruce inner bark extract as a sun protection agent in sunscreens. Ultrasound-assisted extraction with 60 v-% ethanol was applied to isolate the extract in 25-30 % yield, that was almost independent of the temperature (45-75oC) and time (5-60 min) of the treatment. However, the yield of stilbene glucosides, measured by UV absorption spectroscopy, was highest after ca. 20 min extraction. Nuclear magnetic resonance spectroscopy of the extract showed that it consisted mainly of three stilbene glucosides, astringin, isorhapontin and polydatin (piceid). The maximum overall yield of the stilbene glucosides was > 20 %. Extraction with water gave a much lower yield of the stilbene glucosides. Sunscreens composed of a mixture of vegetable oils, surfactants (fatty acids), glycerin, water and the bark extract were prepared with the low-energy emulsification method. The performance of the sunscreens was assessed by spreading them on a photosensitive paper and observing the change in color during exposure to light. Commercial sunscreens with known SPF values (15-50) were used as references. Addition of 2-5 % of the bark extract in the sunscreen provided similar protection against UV light compared to the commercial products. Use of the spruce inner bark extract as the sun protection agent in sunscreens appeared to be potentially feasible and should be studied further. Keywords: Spruce bark; Stilbenes; Ultrasound-Assisted Extraction; UV-Vis; NMR II Contents ABSTRACT .................................................................................................................................... II Contents ......................................................................................................................................... III List of Figures ................................................................................................................................. V List of Tables ................................................................................................................................. VI Symbols and abbreviations ........................................................................................................... VII Symbols ..................................................................................................................................... VII Abbreviations ............................................................................................................................ VII Preface.......................................................................................................................................... VIII 1 Introduction .................................................................................................................................. 1 2 Research objectives ...................................................................................................................... 3 3 Literature review .......................................................................................................................... 4 3.1 Spruce bark ............................................................................................................................ 4 3.1.1 Structure.......................................................................................................................... 4 3.1.2 Chemical composition .................................................................................................... 4 3.1.3 Utilization ....................................................................................................................... 5 3.2 Stilbenes ................................................................................................................................ 6 3.2.1 Structure and chemical composition............................................................................... 6 3.2.2 Seasonal and position variation ...................................................................................... 7 3.2.3 Properties ........................................................................................................................ 7 3.2.3.1 Storage .................................................................................................................... 7 3.2.3.2 Solubility ................................................................................................................. 8 3.2.3.3 Stability ................................................................................................................... 8 3.2.3.4 Anti – UV ability .................................................................................................... 9 3.3 Extraction and isolation methods .......................................................................................... 9 3.4 Utilization in sunscreens and health care ............................................................................ 12 4 Materials and methods ............................................................................................................... 13 4.1 Materials .............................................................................................................................. 13 4.1.1 Source of raw materials ................................................................................................ 13 4.1.2 Raw material preparation .............................................................................................. 13 III 4.2 Methods ............................................................................................................................... 14 4.2.1 Ultrasound-Assisted Extraction .................................................................................... 15 4.2.2 Analytical techniques ................................................................................................... 16 4.2.2.1 UV-Vis spectroscopy ............................................................................................ 16 4.2.2.2 Nuclear Magnetic Resonance spectroscopy .......................................................... 17 4.2.2.3 Chemical composition .......................................................................................... 18 4.2.3 Sunscreen preparation ................................................................................................... 22 4.2.3.1 Raw material selection .......................................................................................... 22 4.2.3.2 Production ............................................................................................................. 23 4.2.3.3 Properties .............................................................................................................. 24 4.2.3.4 Sun protection test................................................................................................. 25 5 Results and discussion ............................................................................................................... 26 5.1 Chemical composition of inner bark ................................................................................... 26 5.2 Quantification of stilbenes by UV-Vis absorption spectroscopy ........................................ 28 5.2.1 Calibration curve .......................................................................................................... 28 5.2.2 Yield of extract and stilbenes ....................................................................................... 30 5.2.3 Stability ......................................................................................................................... 31 5.2.4 Solvent comparison ...................................................................................................... 32 5.3 Quantification by NMR spectroscopy ................................................................................. 33 5.4 Sun protection ability .......................................................................................................... 36 5.4.1 Stability ......................................................................................................................... 37 5.4.2 Cost ............................................................................................................................... 38 6 Conclusions ................................................................................................................................ 39 7 Future research topics ................................................................................................................ 39 Reference .....................................................................................................................................