INDEX
CHAPTER I
1.INTRODUCTION………..……….. 1
1.1. Plant polyphenols………..……… 3
1.2.Analytical methods in the phytochemical studies…... 5
1.3. The Nuclear Magnetic Resonance………...…………. 7
1.4.The aim of the thesis………..……… 8
CHAPTER II
2.MATERIALS AND METHODS……….………...…… 112.1.Standards and solvents…………..……… 13
2.2.General experimental procedures...……..…………... 13
2.2.1. TLC... 13
2.2.2. Gel filtration chromatography... 14
2.2.3. HPLC semipreparative separations... 15
2.2.4. NMR analyses... 15
2.2.5. Mass spectrometry analyses... 16
2.3.HPLC-PDA-ESI-MS analyses... 16
2.3.1. Qualitative analyses... 16
2.3.2. Quantitative analyses... 16
CHAPTER III
3.PHENOLICS OF ARBUTUS UNEDO L.(ERICACEAE)FRUITS: IDENTIFICATION OF ANTHOCYANINS AND GALLIC ACID DERIVATIVES... 173.1.MATERIALS AND METHODS... 20
3.1.1. Plant material... 20
3.1.2. HPLC-PDA-ESI-MS analyses of anthocyanins... 21
3.1.3. Extraction and identification of anthocyanins... 22
3.1.4. Calibration, quantification, and statistical analyses of anthocyanins... 22
3.1.5. Extraction, isolation, and identification of other phenolics... 23
3.2. Results and discussion... 26
3.2.1. Qualitative-quantitative anthocyanins profile... 26
3.2.2. Gallic acid derivatives... 31
CHAPTER IV
4.FLAVONOIDS OF ZIZYPHUS JUJUBA MILL. AND ZIZYPHUS SPINA-CHRISTI (L.)WILLD (RHAMNACEAE)FRUITS... 334.1.MATERIALS AND METHODS... 36
4.1.1. Plant material... 36
4.1.2. HPLC-PDA-ESI-MS analyses... 36
4.1.3. Extraction, isolation, and identification... 37
4.1.4. Quantitative analyses... 42
4.2. Results and discussion... 43
4.2.1. Isolation and structure determination... 43
4.2.2. HPLC-PDA-ESI-MS analyses... 45
4.2.3. Comparative study of flavonoids of Z. jujuba and Z. spina-christi fruits... 50
CHAPTER V
5.QUALI-QUANTITATIVE ANALYSES OF FLAVONOIDS OF MORUS NIGRA L. AND MORUS ALBA L.(MORACEAE) FRUITS... 535.1.MATERIALS AND METHODS... 57
5.1.2. HPLC-PDA-ESI-M analyses... 57
5.1.3. Extraction, isolation, and identification of flavonoids... 58
5.1.4. Extraction and identification of anthocyanins... 61
5.1.5. Quantitative analyses... 61
5.2. Results and discussion... 62
5.2.1. Isolation and structure determination of compounds 1-4... 62
5.2.2. Comparative study of the composition of flavonoids of M. nigra and M. alba fruits... 64
5.2.3. Quali-quantitative anthocyanins profile... 67