New methodologies for the analysis of phytosterols and their intact esters: applications to cereals, nuts and edible plant oils
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| 1. Verfasser: | |
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| Format: | Abschlussarbeit Buch |
| Sprache: | English |
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2014
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| Schlagworte: | |
| Online-Zugang: | kostenfrei https://nbn-resolving.org/urn:nbn:de:bvb:91-diss-20140730-1229692-0-6 Inhaltsverzeichnis |
| Beschreibung: | XI, 177 S. graph. Darst. |
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| 245 | 1 | 0 | |a New methodologies for the analysis of phytosterols and their intact esters |b applications to cereals, nuts and edible plant oils |c Rebecca Esche |
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| adam_text | TECHNISCHE UNIVERSITAT MUNCHEN
LEHRSTUHL FUR ALLGEMEINE LEBENSMITTELTECHNOLOGIE
NEW METHODOLOGIES FOR THE ANALYSIS OF PHYTOSTEROLS AND
THEIR INTACT ESTERS: APPLICATIONS TO CEREALS, NUTS AND
EDIBLE PLANT OILS
REBECCA ESCHE
VOLLSTANDIGER ABDRUCK DER VON DER FAKULTAT WISSENSCHAFTSZENTRUM
WEIHENSTEPHAN FUR
ERNAHRUNG, LANDNUTZUNG UND UMWELT DER TECHNISCHEN UNIVERSITAT MUNCHEN
ZUR ERLANGUNG
DES AKADEMISCHEN GRADES EINES
DOKTORS DER NATURWISSENSCHAFTEN
{DR. RER. NAT]
GENEHMIGTEN DISSERTATION.
VORSITZENDER: UNIV.-PROF. DR. PETER SCHIEBERLE
PRUFER DER DISSERTATION: 1. UNIV.-PROF. DR. KARL-HEINZ ENGEL
2. APL. PROF. DR. PETER K&HLER
DIE DISSERTATION WURDE AM 19.03.2014 BEI DER TECHNISCHEN UNIVERSITAT
MFLNCHEN EINGEREICHT
UND DURCH DIE FAKULTAT WISSENSCHAFTSZENTRUM WEIHENSTEPHAN FUR ERNAHRUNG,
LANDNUTZUNG
UND UMWELT AM 12.06.2014 ANGENOMMEN.
HTTP://D-NB.INFO/1058381946
TABLE OF CONTENTS
TABLE OFCONTENTS
1 INTRODUCTION AND OBJECTIVES 1
2 BACKGROUND 3
2.1 PHYTOSTEROLS/-STANOLS AND THEIR CONJUGATES**.3
2.1.1 STRUCTURAL PROPERTIES, BIOSYNTHESIS, AND BIOLOGICAL FUNCTION IN
PLANTS 3
2.1.2 METABOLISM 7
2.1.3 HEALTH BENEFITS 9
2.2 NATURAL SOURCES OF PHYTOSTEROLS/-STANOLS AND PHYTOSTERYL/-STANYL
ESTERS 14
2.2.1 ESTIMATED INTAKES OFPHYTOSTEROLS/-STANOLS VIA NATURAL SOURCES 14
2.2.2 PHYTOSTEROLS/-STANOLS AND PHYTOSTERYL/-STANYL ESTERS IN CEREALS 14
2.2.2.1 CORN 15
2.2.2.2 SMALL MILLETS AND SORGHUM 16
2.2.2.3 OTHER CEREALS (RYE, WHEAT, AND SPELT) 18
2.2.3 PHYTOSTEROLS/-STANOLS AND PHYTOSTERYL/-STANYL ESTERS IN TREE NUTS
AND PEANUTS 20
2.2.4 PHYTOSTEROLS/-STANOLS AND PHYTOSTEIYL/-STANYL ESTERS IN PLANT OILS
22
2.3 ANALYTICAL METHODS ... 26
2.3.1 ANALYSIS OFTOTAL PHYTOSTEROLS/-STANOLS AND INTACT
PHYTOSTERYL/-STANYL ESTERS 26
2.3.2 PRINCIPLES AND APPLICATION OF ON-LINE LC-GC_..._ ... _28
3 MATERIALS AND METHODS 30
3.1.1 CHEMICALS 30
3.1.2 SYNTHESIS OF REFERENCE COMPOUNDS 31
3.1.2.1 SYNTHESIS OF STERYL/STANYL FATTY ACID ESTERS...* *31
3.1.2.2 SYNTHESIS OF STERYL/STANYL PHENOLIC ACID ESTERS 32
3.1.3 PLANT MATERIALS 33
3.2 METHODS 38
3.2.1 SAMPLE PREPARATION 38
3.2.1.1 PREPARATION OF CEREALS 38
3.2.1.2 PREPARATION OF TREE NUTS AND PEANUTS... ... __ ... _. _ 38
3.2.2 DETERMINATION OF DRY MATTER AND MOISTURE 38
3.2.3 LIPID EXTRACTION 39
3.2.3.1 LIPID EXTRACTION OF CEREAL FLOURS 39
3.2.3.2 LIPID EXTRACTION OF GROUND TREE NUTS AND PEANUTS 39
3.2.4 SOLID-PHASE EXTRACTION AND GC ANALYSIS OF FREE STEROLS/STANOLS AND
STERYL/STANYL
ESTERS I 40
3.2.4.1 SOLID-PHASE EXTRACTION 40
I
TABLE OF CONTENTS
3.2.4.2 GC-FID ANALYSIS 40
3.2.4.3 QUANTIFICATION BY GC-FID 41
3.2.4.4 IDENTIFICATION BY GC-MS 41
3.2.4.5 VALIDATION OF THE SPE-BASED APPROACH ....41
3.2.5 ON-LINE LC-GC ANALYSIS
OF FREE STEROLS/STANOLS AND STERYL/STANYL ESTERS 42
3.2.5.1 SAMPLE PREPARATION 42
3.2.5.2 ON-LINE LC-GC-FID ANALYSIS 43
3.2.5.3 QUANTIFICATION BY ON-LINE LC-GC-FID
* .. ~43
3.2.5.4 IDENTIFICATION BY ON-LINE LC-GC-MS 44
3.2.5.5 VALIDATION OF THE ON-LINE LC-GC-BASED APPROACH 45
3.2.6 GC ANALYSIS OF FATTY
ACID METHYL ESTERS (FAME) - ... ... 46
3.2.6.1 PREPARATION OF FAME 46
3.2.6.2 GC-FID ANALYSIS 47
3.2.6.3 GC-MS ANALYSIS 47
3.2.7 DATA ANALYSIS 47
4 RESULTS AND DISCUSSION 48
4.1 METHOD DEVELOPMENT FOR THE ANALYSIS OF FREE STEROLS/STANOLS AND
INTACT
STERYL/STANYL ESTERS * * 48
4.1.1 ESTABLISHMENT AND VALIDATION OF AN APPROACH BASED ON SPE AND GC
.48
4.1.1.1 SPE AND GC ANALYSIS 48
4.1.1.2 VALIDATION OF THE SPE AND GC-BASED APPROACH 50
4.1.2 ESTABLISHMENT AND VALIDATION OF AN APPROACH BASED ON ON-LINE LC-GC
51
4.1.2.1 ON-LINE LC-GC ANALYSIS ....51
4.1.2.2 VALIDATION OF THE ON-LINE LC-GC-BASED APPROACH .54
4.1.3 IDENTIFICATION OF COMPOUNDS VIA ON-LINE LC-GC-MS 55
4.1.4 COMPARISON OF METHODS 57
4.1.5 SUMMARY. 58
4.2 ANALYSIS OF FREE STEROLS/STANOLS AND STERYL/STANYL ESTERS IN VARIOUS
DENT CORN
AND FLINT COM CULTIVARS ** ~ 59
4.2.1 COMPOSITIONS AND CONTENTS OF FREE STEROLS/STANOLS AND
STERYL/STANYL ESTERS 59
4.2.2 DISTRIBUTION PATTERNS OF FREE AND ESTERIFIED STEROLS/STANOLS 68
4.2.3 DISTRIBUTION PATTERNS OF TOTAL FATTY ACIDS AND OF FATTY ACIDS
ESTERIFIED TO
STEROLS/STANOLS...*. * 68
4.2.4 PROPORTIONS OF FREE STEROLS/STANOLS AND STERYL/STANYL ESTERS 69
4.2.5 COMPARISON OF DENT COM AND FLINT CORN ..... 70
II
TABLE OF CONTENTS
4.3 ANALYSIS OF FREE STEROLS/STANOLS AND STERYL/STANYL ESTERS IN SWEET
COM AND
POPCORN 71
4.3.1 COMPOSITIONS AND CONTENTS OF FREE STEROLS/STANOLS AND
STERYL/STANYL ESTERS 71
4.3.2 DISTRIBUTION PATTERNS OF FREE AND ESTERIFIED STEROLS/STANOLS 75
4.3.3 DISTRIBUTION PATTERNS OF TOTAL FATTY ACIDS AND OF FATTY ACIDS
ESTERIFIED TO
STEROLS/STANOLS 75
4.3.4 PROPORTIONS OF FREE STEROLS/STANOLS AND STERYL/STANYL ESTERS 75
4.4 ANALYSIS OF FREE STEROLS/STANOLS AND STERYL/STANYL ESTERS IN SMALL
MILLETS AND
SORGHUM 77
4.4.1 ON-LINE LC-GC-BASED APPROACH 77
4.4.2 COMPOSITIONS AND CONTENTS OF FREE STEROLS/STANOLS AND
STERYL/STANYL ESTERS 78
4.4.3 DISTRIBUTION PATTERNS OF FREE AND ESTERIFIED STEROLS/STANOLS 90
4.4.4 DISTRIBUTION PATTERNS OF TOTAL FATTY ACIDS AND OF FATTY ACIDS
ESTERIFIED TO
STEROLS/STANOLS 90
4.4.5 PROPORTIONS OF FREE STEROLS/STANOLS AND STERYL/STANYL ESTERS 91
4.5 ANALYSIS OF FREE STEROLS/STANOLS AND STERYL/STANYL ESTERS IN RYE,
WHEAT, AND
SPELT 93
4.5.1 COMPOSITIONS AND CONTENTS OF FREE STEROLS/STANOLS AND
STERYL/STANYL ESTERS 94
4.5.2 DISTRIBUTION PATTERNS OF FREE AND ESTERIFIED STEROLS/STANOLS 99
4.5.3 DISTRIBUTION PATTERNS OF TOTAL FATTY ACIDS AND OF FATTY ACIDS
ESTERIFIED TO
STEROLS/STANOLS 99
4.5.4 PROPORTIONS OF FREE STEROLS/STANOLS AND STERYL/STANYL ESTERS 99
4.6 ANALYSIS OF FREE STEROLS/STANOLS, STERYL/STANYL ESTERS, AND OTHER
MINOR LIPIDS IN
TREE NUTS AND PEANUTS - 101
4.6.1 ON-LINE LC-GC-BASED APPROACH 101
4.6.2 COMPOSITIONS AND CONTENTS OF FREE STEROLS/STANOLS AND
STERYL/STANYL ESTERS.*. 102
4.6.3 DISTRIBUTION PATTERNS OF FREE AND ESTERIFIED STEROLS/STANOLS 110
4.6.4 DISTRIBUTION PATTERNS OF TOTAL FATTY ACIDS AND OF FATTY ACIDS
ESTERIFIED TO
STEROLS/STANOLS 110
4.6.5 PROPORTIONS OF FREE STEROLS/STANOLS AND STERYL/STANYL ESTERS 111
4.6.6 TOCOPHEROLS AND SQUALENE ; 112
4.7 ANALYSIS OF FREE STEROLS/STANOLS, STERYL/STANYL ESTERS AND OTHER
MINOR LIPIDS IN
EDIBLE PLANT OILS _._..._
U
*.._.__..__....__..115
4.7.1 ON-LINE LC-GC-BASED APPROACH 115
4.7.2 COMPOSITIONS AND CONTENTS OF FREE STEROLS/STANOLS AND
STERYL/STANYL ESTERS 116
4.7.3 DISTRIBUTION PATTERNS OF FREE AND ESTERIFIED STEROLS/STANOLS 128
III
TABLE OF CONTENTS
4.7.4 DISTRIBUTION PATTERNS OF TOTAL FATTY ACIDS AND OF FATTY ACIDS
ESTERIFIED TO
STEROLS/STANOLS 128
4.7.5 PROPORTIONS OF FREE STEROLS/STANOLS AND STERYL/STANYL ESTERS 129
4.7.6 TOCOPHEROLS, SQUALENE, AND FREE FATTY ACIDS 131
4.7.7 COMPARISON OF NATIVE AND REFINED OILS 134
4.8 COMPARISON OF CEREALS, NUTS, AND EDIBLE PLANT OILS 136
5 SUMMARY I 139
6 ZUSAMMENFASSUNG 141
7 REFERENCES 144
8 APPENDIX 166
9 PUBLICATIONS AND PRESENTATIONS. 175
10 CURRICULUM VITAE 177
IV
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| spelling | Esche, Rebecca Verfasser aut New methodologies for the analysis of phytosterols and their intact esters applications to cereals, nuts and edible plant oils Rebecca Esche 2014 XI, 177 S. graph. Darst. txt rdacontent n rdamedia nc rdacarrier München, Techn. Univ., Diss., 2014 Zsfassung in dt. Sprache (DE-588)4113937-9 Hochschulschrift gnd-content Erscheint auch als Online-Ausgabe urn:nbn:de:bvb:91-diss-20140730-1229692-0-6 https://mediatum.ub.tum.de/node?id=1229692 Verlag kostenfrei Volltext https://nbn-resolving.org/urn:nbn:de:bvb:91-diss-20140730-1229692-0-6 Resolving-System DNB Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=027501685&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis |
| spellingShingle | Esche, Rebecca New methodologies for the analysis of phytosterols and their intact esters applications to cereals, nuts and edible plant oils |
| subject_GND | (DE-588)4113937-9 |
| title | New methodologies for the analysis of phytosterols and their intact esters applications to cereals, nuts and edible plant oils |
| title_auth | New methodologies for the analysis of phytosterols and their intact esters applications to cereals, nuts and edible plant oils |
| title_exact_search | New methodologies for the analysis of phytosterols and their intact esters applications to cereals, nuts and edible plant oils |
| title_full | New methodologies for the analysis of phytosterols and their intact esters applications to cereals, nuts and edible plant oils Rebecca Esche |
| title_fullStr | New methodologies for the analysis of phytosterols and their intact esters applications to cereals, nuts and edible plant oils Rebecca Esche |
| title_full_unstemmed | New methodologies for the analysis of phytosterols and their intact esters applications to cereals, nuts and edible plant oils Rebecca Esche |
| title_short | New methodologies for the analysis of phytosterols and their intact esters |
| title_sort | new methodologies for the analysis of phytosterols and their intact esters applications to cereals nuts and edible plant oils |
| title_sub | applications to cereals, nuts and edible plant oils |
| topic_facet | Hochschulschrift |
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