CHARACTERIZATION OF DESERT DATE (Balanites aegyptiaca)

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experiment gave a drastically reduced free sugar peak. This experiment was undertaken to collect the individual peak saponins. Mass spectrometry All the experiments were performed with a single-ion-trap mass spectrometer (Esquire 3000 Plus, Bruker Daltonik, Germany) equipped with an ESI interface as the ion source for MS analyses. The electrospray voltage was set at 4.5 kV. The temperature of the ion source capillary was 300ºC. Negative ion mode was used for all experiments. Mass spectrometer conditions were optimized to achieve maximum sensitivity. Full scan spectra from m/z 25 to 2000 in the negative ion mode were obtained (scan time 1 s). The ion trap was set for acquisition in automatic gain control mode with an accumulation time of 159 µs. For MS n analyses, the isolation width for [M-H] - molecular ions was 3 m/z units; for MS n experiments, fragmentation was induced using activation amplitudes of 0.95 to 1.12 V. NMR spectrometry 1 13 o H, C, and DEPT 135 NMR spectra were recorded at 25 C with a Varian Unity Inova 800 spectrometer (proton frequency 799.809 MHz) in CD3OD with TMS as internal reference. NOESY spectra were obtained with mixing times of 700 ms. HMBC experiments were optimized for n JC,H = 5 Hz. Mass spectra were obtained on a JEOL JMS- AX505W double-focusing mass spectrometer operating in EI mode. The NMR study was carried out in the Danish University of Pharmaceutical Sciences, Copenhagen, Denmark. Results Analysis of B. aegyptiaca mesocarp extracts by LC-MS Figure 2.1 shows the HPLC (RI) and MS total-ion-current (TIC) chromatograms of the methanol extracts of B. aegyptiaca mesocarp (ME). There are eight separation peaks at 4.2, 4.8, 6.0, 7.2, 8.2, 8.6, 11.2, and 12.4 min retention time in HPLC-RI. There is a large void volume at the beginning of the chromatogram, perhaps due to the free sugar compounds in the B. aegyptiaca mesocarp (Figure 2.1a). However, this large void volume was drastically reduced when the extract was further eluted by water, using an SPE Sep-Pak C18 cartridge 19
and analysed with an ELS detector (Figure 2.1b). A clear correlation between the peaks obtained from the RI (HPLC chromatogram) and the MS (TIC chromatogram) are also observed. A comparison of the ELS and RI chromatograms revealed a very similar pattern of peaks; however, the retention times were different. Since the ELS detector was not coupled to the MS, further analysis of each MS peak was carried out with an RI detector. The ESI mass spectra [M-H] - of each of the eight RI peaks are presented in Figure 2.2, with their corresponding retention times. A summary of the peaks with retention time, m/z value [M-H] - , and area is also listed in Table 2.1. Among the eight peaks there are actually only five masses, m/z 1195, 1063, 1077, 1209, and 1045, in negative ion mode (Table 2.1). The ion at m/z 1077 repeated three times: at 6.0, 8.2, and 11.2 min; the ion at m/z 1209 repeated twice: at 7.2 and 9.6 min. An estimated quantification shows that the m/z 1063 peak at 4.8 min retention time is the largest, corresponding to 18.75%, followed by peaks at m/z 1209 (11.8%), 1077 (10.89%), 1045 (1.55%), and 1195 (1.35%) of the injected sample. 20
Page 1 and 2: CHARACTERIZATION OF DESERT DATE (Ba
Page 3 and 4: This work was carried out under the
Page 5 and 6: Abstract The desert date (Balanites
Page 7 and 8: of various Balanites tissues sugges
Page 9 and 10: Contents Acknowledgements i Abstrac
Page 11 and 12: Materials and methods 38 - Sample c
Page 13 and 14: - Effect of the saponin source on p
Page 15 and 16: Figure 2.9 1 H NMR spectrum showing
Page 17 and 18: List of Tables Table 2.1 Major HPLC
Page 19 and 20: Glossary CID collision induced diss
Page 21 and 22: Thesis organization This thesis is
Page 23 and 24: fruits have been found in Pharaohs'
Page 25 and 26: Fig 1.3. Map showing the Balanites
Page 27 and 28: themselves provide shade and shelte
Page 29 and 30: should be no surprise that the name
Page 31 and 32: Association with membranes Most bio
Page 33 and 34: the African or Indian samples. No w
Page 35 and 36: Objective and Hypothesis Objectives
Page 37 and 38: CHAPTER 2 Characterization of the f
Page 39: Extraction and separation For the e
Page 43 and 44: c d a Figure 2.2. Electrospray mass
Page 45 and 46: corresponds with the claims of earl
Page 47 and 48: Table 2.2. MS n Electrospray mass s
Page 49 and 50: 1209, and could be isomers of these
Page 51 and 52: compound as 26-(O-β-D-glucopyranos
Page 53 and 54: In the 1 H NMR spectrum, resonances
Page 55 and 56: Figure 2.11. Structure of the sapon
Page 57 and 58: Conclusions From this study we can
Page 59 and 60: that a study of the saponin profile
Page 61 and 62: HPLC pump and a refractive index (R
Page 63 and 64: Table 3.1 Peaks, retention time, am
Page 65 and 66: (a) (b) (c) (d) (e) Figure 3.2 ESI-
Page 67 and 68: Table 3.2 The LC-ESI-MS and corresp
Page 69 and 70: quoted here also are integers obtai
Page 71 and 72: (a) (b) (c) (d) (e) (f) (g) (i) Fig
Page 73 and 74: considered cleavage behavior, from
Page 75 and 76: Table 3.4 The LC-ESI-MS and corresp
Page 77 and 78: The results of this study also show
Page 79 and 80: ich extracts of Agave sisalana (Piz
Page 81 and 82: food preparation based on baby food
Page 83 and 84: Table 4.3 LC50 and LC90 (ppm) of sa
Page 85 and 86: 1 2 3 Figure 4.1 Structure of the t
Page 87 and 88: When the images of dead larvae were
Page 89 and 90: CHAPTER 5 Antifungal activity of sa
Page 91 and 92:
visually and microscopically, and s
Page 93 and 94:
Effects of the SREs on in vitro gro
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Table 5.2 Effect of saponin rich ex
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(Table 5.3). In the case of C. cocc
Page 99 and 100:
CHAPTER 6 Effect of saponins on del
Page 101 and 102:
astomatous cuticles from the upper
Page 103 and 104:
Results Effect of the saponin sourc
Page 105 and 106:
Effect of humidity and temperature
Page 107 and 108:
Table 6.3 Effect of humidity and te
Page 109 and 110:
Discussion and conclusions Agro-mat
Page 111 and 112:
solutions used in our studies has s
Page 113 and 114:
CHAPTER 7 General conclusions and s
Page 115 and 116:
as a delivery adjuvant, not only in
Page 117 and 118:
Botanic Gardens, Kew. 960 pp. Bushw
Page 119 and 120:
Ganzera, M., Bedir, E., Khan ,I.A.
Page 121 and 122:
Keukens, E.A.J., de Vrije, T., van
Page 123 and 124:
Morrissey, J.P., Osbourn, A.E. (199
Page 125 and 126:
Schonherr, J., Riederer, M. (1986).
Page 127 and 128:
Appendices A1 - A4: Articles publis
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new and alternative sources of thes
Page 131 and 132:
first dissolved in 1 ml methanol an
Page 133 and 134:
In Table 1, the total sapogenin as
Page 135 and 136:
114 5. Beneytout JL, Nappez C, Lebo
Page 137 and 138:
Appendix: A2 Natural Product Commun
Page 139 and 140:
min, and finally rinsed three times
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level was significantly increased f
Page 143 and 144:
Table1. Effect of plant growth regu
Page 145 and 146:
A B C D Fig 1. Different callus typ
Page 147 and 148:
Appendix: A3 African Journal of Bio
Page 149 and 150:
The data obtained were statisticall
Page 151 and 152:
Table 4. Mortality of Culex pipiens
Page 153 and 154:
Appendix: A4 Dengue Bulletin 2005;
Page 155 and 156:
of the Institutes for Applied Resea
Page 157 and 158:
References 136 1. Halstead SB. Glob
Page 159 and 160:
112 H20a-H21-H23b-H24bb 23a 31.5 1.
Page 161 and 162:
112.0 H15 β -H17a-H20a-H21 23a 31.
Page 163 and 164:
112 H20b-H24aa-H24bb 23a 31.4 1.64
Page 165 and 166:
םהיתויוליעפו םהיתו
Page 167 and 168:
. םיינגוזה םורדו תח
Page 169 and 170:
םוקאזה ישרושב ירקי
Page 171:
םיטביה לש הנבהה היי
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CHARACTERIZATION OF DESERT DATE (Balanites aegyptiaca)

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