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Dataset on the Microstructural and Microchemical Characterization of Valorized Cola nitida Pod Wastes
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Dataset on the Microstructural and Microchemical Characterization of Valorized Cola nitida Pod Wastes Olalere Olusegun Abayomi , Chee-Yuen Gan , Abdurahman Hamid Nour , Muhammad Sheraz Ahmad , Aziz Qannaf Zaid , Omar Abed Habeeb PII: DOI: Reference:
S2405-8300(20)30067-7 https://doi.org/10.1016/j.cdc.2020.100356 CDC 100356
To appear in:
Chemical Data Collections
Received date: Revised date: Accepted date:
17 October 2019 28 January 2020 13 February 2020
Please cite this article as: Olalere Olusegun Abayomi , Chee-Yuen Gan , Abdurahman Hamid Nour , Muhammad Sheraz Ahmad , Aziz Qannaf Zaid , Omar Abed Habeeb , Dataset on the Microstructural and Microchemical Characterization of Valorized Cola nitida Pod Wastes, Chemical Data Collections (2020), doi: https://doi.org/10.1016/j.cdc.2020.100356
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Dataset on the Microstructural and Microchemical Characterization of Valorized Cola nitida Pod Wastes Olalere Olusegun Abayomi1*, Chee-Yuen Gan1*, Abdurahman Hamid Nour2, Muhammad Sheraz Ahmad 2, Aziz Qannaf Zaid2, Omar Abed Habeeb2 1
Analytical Biochemistry Research Center (ABrC), Universiti Sains Malaysia (USM), 11800 Gelugor, Penang, Malaysia 2
Chemical and Process Engineering. Universiti Malaysia Pahang (UMP), 26300, Gambang, Malaysia Corresponding author: [email protected] (Gan C.Y.) ; [email protected] (Olalere O.A.) Abstract The inherent environmental effects of the accumulated kola nut pod waste products have become a subject of discussion among many researchers. The need then arises for their alternative use as nutraceutical bioproducts. The physical and chemical analytical techniques are often required for the standardization of these bioproducts in order to determine and maintain their quality characteristics. The dataset presented in this study provided information on the chemical profile, physisorption and thermo-analytical screening of Cola nut pod extracts. Six sets of physicochemical methods were employed to characterize the phenolic extracts. The result obtained clearly revealed the presence of two-hundred and fifty-five phenolic bioactive. Also presented was the thermal stability, morphological and microstructural surface area configuration of the Cola nitida pod extracts. The information obtained from this study could be used in determining the quality of food wastes bioproducts in nutria-pharmaceutical applications. Keywords: Brunauer-Emmett-Teller (BET), Cola nitida; Differential scanning calorimetry (DSC), Thermogravimetry analysis (TGA)
Specification Table Subject area More specific subject area Type of data How data was acquired
Microchemical science Food characterization Table, Figure, Spectra a) The dataset was acquired for both positive and negative ESI-mode using LC-MS/QToF (Waters, USA). b) Thermo-analytical elucidation using TGA (Model Q500-V6.4, Germany) and DSC scanning calorimeter (model-NETZSCH DSC 214) c) Surface area elucidation using BrunauerEmmett-Teller (BET)
Data accessibility
d) Functional group characteristics using the Thermo-Nicolet spectrometer (iS5 iD7-ATR, Germany). The dataset consisting of tables, spectra, and figures can be found along with the article
1. Rationale The inherent hazard of agricultural wastes to the environment necessitates their conversion to useful-bioproducts [1]. The polyphenolic constituents of kola nut pod are widely applied in food, biopharmaceutical, and petrochemical industries. The need then arises for a physicochemical analysis that will ensure and monitor the nutritional and medicinal quality of the bioproducts from physical and chemical degradation [2]. The dataset presented a succinct microstructural, microchemical and thermophysical characterization of C.nitida pod extracts. The data consists of the phenolic profiles (Table 1) of the C.nitida oleoresin extracts obtained from the Liquid chromatography-QToF Spectrometer (LC-MS/QToF). The dried extracts were characterized to determine the effect of electromagnetic waves from microwave extractor on the thermal stability, functional group characteristics, morphological features and microstructural surface area using Thermogravimetry analyzer (TGA), Differential scanning calorimetry (DSC), Fourier transform infrared (FTIR), Field emission scanning electron microscopy (FESEM) and Brunauer-Emmett-Teller (BET). 2. Procedure 2.1 Raw material preparation The kola nut pods wastes were harvested, air-dried, crushed and sieved into particle size (< 0.50 mm) using a set of standard sieves. The extract was prepared using the microwave extractor (Ethos Milestone, USA) operated in a three-level temperature setting. The first set involves the use of moderate heat (40 °C) to trigger off the induction process which helps in breaking up the cellulosic cell wall of the sample. The second setting involves the extraction temperature (60 °C), while the last stage involves the cooling stage. The C. nitida was loaded into the microwave reactor and the bioproduct was extracted at the microwave power of 450 W, the irradiation time of 5 min, using 60 % ethanol as extracting solvent [3]. After extraction, the resulting bioproduct was unloaded from the microwave reactor and filtered using a vacuum pump (VP250N, Zhejiang, China). The filtrate was thereafter evaporated at 78 °C under vacuum to obtain a semisolid oleoresin extract, which was later subjected to spray-drying and refrigerated for further microchemical characterization and surface probes. 2.2 LC-MS chemical profiling The C. nitida oleoresin extracts were analyzed using Vion Ion Mobility QTOF MS, Waters, (USA) with the aid of an ACQUITY UPLCHSS-T3 column 2.1 x 100 mm and particle size 1.8 mm). The extract was pre-treated and the concentration adjusted to 20 ppm before injection into the LC–MSQ- the time of flight mass spectrometer according to the method employed by Olalere et al., [4]. The peak of parent and daughter fragmentation of different components was identified using a negative electron-spray ionization mode [5].
2.3 Fourier transformed infrared spectroscopy (FT-IR) The Fourier Transform Infrared (FTIR) spectroscopic analysis was conducted according to Olalere et al., [6].The functional group characteristics of the dried C. nitida powder was determined using a Thermo-Nicolet spectrometer (iS5 iD7-ATR, Germany). The spectra interpretation was performed with the aid of a Thermoscienctific OMNIC software (Vs. 9.0). The minimum and maximum range of the wavenumber was 500 cm-1 and 4000 cm-1. 2.4 Thermogravimetry analysis (TG) and Differential Scanning Calorimetry (DSC) The TGA curves were generated using an integrated TG-DTA assemblage (Model Q500-V6.4, Germany). The extracts (5.994 mg) were subjected to a temperature range between 30 and 500 °C inside an alumina pan of under atmospheric nitrogen (N2) at a heating rate of 10 °C min-1 and gas flow rate of 20 mL min-1[7]. Moreover, the DSC curves of the C. nitida pod extracts were generated using a thermogravimetric calorimeter (NETZSCH DSC-214 model). The sample mass (5.0 mg) was subjected to atmospheric nitrogen at the flow rate range 40 – 60 mL min -1. The thermal stability test was conducted at a temperature ranging from 25 – 550 °C with a heating rate of 10 K min-1. Moreover, pure indium (m. p. 156 °C) was employed to calibrate the calorimetry analyzer at the standard experimental condition. 2.5 Brunauer-Emmett-Teller (BET) In this study, the BET surface area, pore-volume, and pore size of the C. nitida were measured by nitrogen physisorption at N2 liquefaction temperature of 77 K on a Surfer Thermo Scientific unit. The textural properties of the samples were measured using an accurately weighed 0.5 g of the C. nitida [8]. This was followed by the adsorption/desorption stage involving the degassing of samples in slow mode at 423 K for 3 h. Fast mode degassing was thereafter initiated at 573 K for 12 h to remove the inherent moisture in the sample. The sample was then analyzed in a Dewar flask filled with liquid N2 for physisorption evaluation. The information obtained from the microstructure was analyzed with the aid of a Surfer Acquisition computer software connected to the instrument. 3. Data, value, and validation 3.1 Identification of phenolic content The functional phenolic secondary metabolites in C.nitida were tentatively identified and quantified using mass spectrometry techniques. The results obtained identified a total of 255 phenolic constituents with the major bioactive compounds such as Tribulusamide B (m/z =683.2261) and Cearoin (m/z =289.07). The identified and quantified secondary metabolites are partly responsible for the nutritional and medicinal potential of the valorized C. nitida pod. Table 1 is the output file from LCMS-QToF spectrometer containing the summary of all bioactive phenolic compounds identified with their mass-to-charge ratio, fragmented ions and respective retention time. Table 1: Tentative Phenolic compounds identified in the C. nitida extracts by LCMS-Q-TOF .
Component name
1
DO 19
Observed m/z 585.1785
Observed RT (min) 0.39
Observed CCS (Ų) +HCOO 212.47
Response Adducts 100
Total Fragments Found 1
2
Tribulusamide B
683.2261
0.39
316
+HCOO 184.61
0
3
Tribulusamide B
683.2261
0.39
766
+HCOO 320.24
4
4
Tribulusamide B
683.2261
0.40
6857
+HCOO 266.22
7
5
Tribulusamide B
683.2261
0.40
21588
+HCOO 224.91
6
6
2,3,5,4'Tetrahydroxystilbene-2O-β-Dglucopyranoside Haematoxylin Dihydrooxyresveratrol Euparin Piceatannol Protosappanin C Methyl-5-Ocaffeoylquinate 2,4,6Trihydroxyacetophenon e-2,4-di-O-β-Dglucopyranoside Moracin M Moracin M-3′-O-βD- glucopyranoside p-Tolualdehyde
451.1258
0.40
145
+HCOO 187.47
1
301.0723 245.0822 215.0718 289.0720 301.0721 367.1052
0.40 0.41 0.41 0.41 0.42 0.42
85 912 101 6161 335 934
-H -H -H +HCOO -H -H
238.28 152.49 156.75 152.91 156.30 170.83
0 0 2 0 1 2
491.1404
0.42
221
-H
203.81
0
287.0564 449.1102
0.43 0.44
354 204
+HCOO 157.26 +HCOO 187.21
0 0
167.0353
0.44
167
+HCOO 123.08
0
7 8 9 10 11 12 13
14 15 16
Table 1: Cont’d .
Component name
17
Protocatechuic aldehyde
18 19 20 21 22 23
Sodium ferulate Procyanidin C-1 Dihydrooxyresveratrol Piceatannol p-Tolualdehyde Moracin M-3′-O-β-Dglucopyranoside Koaburaside Piceatannol Vanillin 2,3,5,4'-Tetrahydroxystilbene-2O-β-D-glucopyranoside Protocatechuic aldehyde Protocatechuic aldehyde Protocatechuic aldehyde 2,3,5,4'-Tetrahydroxystilbene-2O-β-D-glucopyranoside
24 25 26 27 28 29 30 31
Observed m/z 137.0242
Observed RT (min) 0.46
-H
Observed CCS (Ų) 122.79
Total Fragments Found 0
215.0326 911.2030 245.0825 289.0717 167.0346 449.1091
352 144 327 3034 218 420
-H +HCOO -H +HCOO +HCOO +HCOO
171.45 268.49 153.74 153.23 124.26 190.69
0 0 0 0 0 0
2.45 2.54 2.70 2.96
117 4633 135 391
-H +HCOO +HCOO +HCOO
168.45 153.51 185.22 189.10
1 0 0 0
3.08 3.16 3.18 3.37
1476 1783 760 334
-H -H -H +HCOO
124.98 120.03 140.94 207.35
0 0 0 0
Response
Adducts
198
0.48 1.96 2.03 2.06 2.07 2.31
331.1028 289.0719 197.0450 451.1241 137.0242 137.0242 137.0242 451.1255
32 33
2,4,6-Trihydroxyacetophenon e-2,4di-O-β-D-glucopyranoside 4-Hydroxyacetophenone
491.1417
3.42
451
-H
206.25
1
135.0448
3.46
1911
-H
130.34
0
Observed m/z 451.1250
Observed RT (min) 3.53
Response
Adducts
337
+HCOO
Observed CCS (Ų) 189.60
Total Fragments Found 0
363.1440 491.1401
3.55 3.63
189 231
+HCOO -H
174.88 205.41
0 0
287.0556 451.1022 451.1240
3.72 3.73 3.75
401 415 362
+HCOO -H +HCOO
223.56 217.75 188.93
0 14 0
451.1247
3.82
1001
+HCOO
187.82
0
401.1434 151.0393 245.0452
3.84 3.89 3.90
88 126 205
+HCOO -H -H
195.16 159.80 165.91
0 0 1
287.0560 271.0611 121.0291 221.0818
3.90 3.91 3.91 3.91
484 259 227 335
+HCOO -H -H -H
199.28 155.97 126.96 144.35
1 10 0 0
287.0561 303.0496 137.0240 289.0718
3.91 3.91 3.91 3.91
719 159 323 29671
225.10 157.95 184.83 153.63
0 2 1 7
245.0818 137.0240
3.92 3.92
5375 440
+HCOO +HCOO -H +HCOO, -H -H -H
152.58 163.62
1 1
Table 1: Cont’d .
Component name
34
48 49 50 51
2,3,5,4'Tetrahydroxystilbene-2O-β-D-glucopyranoside Erianin 2,4,6Trihydroxyacetophenon e-2,4-di-O-β-Dglucopyranoside Moracin M Cinchonain Ia 2,3,5,4'Tetrahydroxystilbene-2O-β-D-glucopyranoside 2,3,5,4'Tetrahydroxystilbene-2O-β-Dglucopyranoside Feroxin A Vanillin 2,4,4′,6′-Tetrahydroxybenzophenone Nobilone Protosappanin A p-Tolualdehyde 4-(4'-Hydroxy-3',5'dimethoxyphenyl)3- buten-2-one Moracin M Dendroflorin Protocatechuic aldehyde Cearoin
52 53
Dihydrooxyresveratrol Sesamol
35 36
37 38 39
40
41 42 43 44 45 46 47
Table 1: Cont’d
.
Component name
54 55 56
Cearoin Pyrogallic acid Nobilone
57
2,4,6-Trihydroxyacetophenon e2,4-di-O-β-D glucopyranoside Dendroflorin 2,3,5,4'-Tetrahydroxystilbene-2O-β-D-glucopyranoside Procyanidin C-1 2,3,5,4'-Tetrahydroxystilbene-2O-β-D-glucopyranoside Cinchonain Ia Moracin F Procyanidin C-1 Brazilein Cinchonain Ia Apocynin B Nobilone 1,2,6-Tri-O-galloyl-β-Dglucopyranoside Cinchonain Ia Procyanidin C-1 2,3,5,4'-Tetrahydroxystilbene-2O-β-D-glucopyranoside Feroxin A Protocatechuic aldehyde 4-(4'-Hydroxy-3',5'dimethoxyphenyl)-3buten-2-one Sesamol Cearoin Cearoin
58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 74 75
76 77 78
Observed m/z 289.0717 125.0242 287.0561
Observed RT (min) 3.92 3.92 3.92
Response
Adducts
2498 316 2846
+HCOO -H +HCOO, -H
Observed CCS (Ų) 222.06 163.23 159.45
491.1418
Total Fragments Found 1 0 2
4.12
417
-H
207.51
0
303.0510 451.1253
4.12 4.22
231 369
+HCOO +HCOO
187.94 185.79
0 0
865.1979 451.1258
4.38 4.41
3502 379
-H +HCOO
270.11 206.88
1 0
451.1024 331.0828 865.1976 329.0678 451.1025 467.0978 287.0553 635.0884
4.50 4.51 4.52 4.53 4.54 4.76 4.82 4.83
425 102 2172 245 692 127 347 133
-H +HCOO -H +HCOO -H -H +HCOO -H
188.17 166.52 266.40 176.24 217.84 230.34 221.55 231.48
3 1 0 0 4 1 1 0
451.1033 865.1975 451.1243
4.83 5.04 5.07
505 1674 2245
-H -H +HCOO
218.99 269.08 188.10
18 1 0
401.1444 137.0241 221.0822
5.13 5.15 5.17
279 274 345
+HCOO -H -H
195.88 124.45 144.80
2 0 0
137.0241 289.0715 289.0715
5.17 5.17 5.17
827 35074 2568
-H +HCOO, -H +HCOO
164.76 153.69 197.56
1 7 2
Table 1: Cont’d .
Component name
79 80 81 82 83 84 85 86
Dihydrooxyresveratrol Dihydrooxyresveratrol Nobilone Moracin M Vanillin Cearoin Pyrogallic acid Dendroflorin
87 88
Protosappanin A 2,4,4′,6′-Tetrahydroxybenzophenone Aspidinol Feroxin A Cinchonain Ia Procyanidin C-1 Caesalpins P Brazilein Protosappanin E-1 2,7-Dihydroxy-1,3-di(phydroxybenzyl)-4methoxy-9,10dihydrophenanthrene Terrestriamide Protosappanin E-1 p-Tolualdehyde Piceatannol Protosappanin A Terrestriamide Apocynin B Procyanidin C-1 Moracin M-3′-O-β-Dglucopyranoside Procyanidin C-1 4-Hydroxyacetophenone Feralolide Moracin F Hematine
89 90 91 92 93 94 95 96
97 98 99 100 101 102 103 104 105 106 107 108 109 110
Observed m/z 245.0818 245.0818 287.0554 287.0554 151.0395 289.0715 125.0242 257.0447
Observed RT (min) 5.17 5.18 5.18 5.18 5.18 5.18 5.18 5.18
-H -H +HCOO, -H +HCOO -H +HCOO -H -H,+HCOO
Observed CCS (Ų) 152.52 217.74 158.90 223.79 160.27 221.67 163.26 154.80
Total Fragments Found 1 0 2 0 0 3 0 4
271.0601 245.0447
236 201
-H -H
156.97 151.08
8 1
5.31 5.31 5.51 5.52 5.53 5.53 5.53 5.54
300 820 439 1437 73 202 233 243
+HCOO +HCOO -H -H -H +HCOO +HCOO -H
197.72 196.48 189.84 262.93 228.75 161.99 239.16 200.07
0 1 1 0 3 0 0 0
372.1090 631.1450 167.0344 289.0712 271.0608 372.1079 467.0996 865.1982 449.1087
5.55 5.59 5.62 5.68 5.69 5.70 5.74 5.74 5.89
291 235 397 1523 210 151 171 3253 8343
+HCOO +HCOO +HCOO +HCOO -H +HCOO -H -H +HCOO
172.33 223.47 126.82 221.38 216.48 170.68 240.19 270.81 190.93
0 1 0 0 0 0 0 1 1
865.1979 135.0446 343.0833 331.0812 299.0547
5.91 5.98 6.11 6.12 6.14
9530 236 219 251 415
-H -H -H +HCOO -H
271.03 129.83 181.27 167.12 164.31
11 0 0 3 2
Response
Adducts
5577 187 3485 1028 126 3935 461 142
5.18 5.18
269.1025 401.1449 451.1037 865.1980 299.0551 329.0659 631.1449 453.1723
Table 1: Cont’d .
Component name
111 112 113 114 115 116 117 118 119 120 121 122 123 124 125 126 127 128 129 130 131 132 133 134 135 136 137 138
Protosappanin C Protosappanin C (R)-Prechrysophanol Protosappanin C Phenol Protosappanin C 3,5,4'-Trihydroxystilbene Euparin Moracin M Caesalpins J Terrestriamide Procyanidin C-1 Apocynin B Terrestriamide Polydatin 3,5,4'-Trihydroxystilbene 3,5,4'-Trihydroxystilbene Polydatin Confusarin Smilaxin Piceatannol Procyanidin C-1 Phenol Protosappanin C Protosappanin C Euparin (R)-Prechrysophanol 7,2′,3′-Trihydroxy-4′methoxy-isoflavan Protosappanin C Caesalpins P Moracin F Blestritin B Brazilein
139 140 141 142 143
Observed m/z 301.0715 301.0714 257.0815 301.0714 139.0401 301.0715 273.0755 215.0713 287.0555 315.0868 372.1094 865.1982 467.0984 372.1087 435.1314 227.0709 227.0709 389.1253 345.0977 315.0868 289.0713 865.1996 139.0396 301.0719 301.0719 215.0713 257.0823 333.0969
Observed RT (min) 6.14 6.14 6.14 6.15 6.15 6.15 6.15 6.15 6.15 6.16 6.34 6.41 6.61 6.79 6.80 6.87 6.88 6.88 6.89 7.01 7.07 7.11 7.13 7.13 7.14 7.14 7.14 7.14
301.0718 299.0556 331.0821 531.2036 329.0666
7.15 7.15 7.15 7.16 7.16
-H -H -H -H +HCOO -H +HCOO -H +HCOO -H +HCOO -H -H +HCOO +HCOO -H -H -H +HCOO -H +HCOO -H +HCOO -H -H -H -H +HCOO
Observed CCS (Ų) 241.22 210.56 156.74 186.62 164.10 155.85 158.67 158.04 223.73 170.08 173.62 275.25 194.57 171.49 198.63 206.92 153.74 203.77 168.22 160.42 224.43 267.65 163.37 202.73 155.80 158.10 156.15 242.44
Total Fragments Found 1 1 2 1 0 6 0 2 0 3 0 1 1 0 0 0 0 1 0 0 0 1 0 1 7 2 3 0
-H -H +HCOO +HCOO +HCOO
240.75 164.68 169.34 221.98 166.69
1 1 1 0 0
Response
Adducts
309 261 664 413 127 4818 164 1430 412 569 337 1153 147 449 166 117 95 86 117 742 1476 1261 159 514 5942 1727 846 100 396 807 560 98 344
Table 1: Cont’d .
Component name
144 145 146 147 148 149 150 151 152 153 154 155 156 157 158 159
Cinchonain Ia Protosappanin A Haematoxylin Protosappanin A Procyanidin C-1 Confusarin Protosappanin A Protosappanin E-1 Protosappanin E-1 Cinchonain Ia Smilaxin Procyanidin C-1 Thannilignan Cinchonain Ia Moracin M 3,7-Dihydroxy-2,4dimethoxyphenanthren e-3-Oglucoside Kuzubutenolide A Protosappanin A Caesalpins J Polydatin Feroxin B Cinchonain Ia Protosappanin A Protosappanin A Caesalpins J Protosappanin A Protosappanin E-1 1,7-Bis(4-hydroxyphenyl)hepta-4E,6E-dien-3-one Smilaxin 3,5,4'-Trihydroxystilbene (-)-Vestitol Caesalpins J (-)-Vestitol Caesalpins J
160 161 162 163 164 165 166 167 168 169 170 171 172 173 174 175 176 177
Observed m/z 451.1036 271.0606 347.0773 317.0661 865.1982 345.0989 317.0666 631.1453 631.1454 451.1039 361.0933 865.1977 329.1407 451.1038 287.0560 477.1413
Observed RT (min) 7.21 7.22 7.26 7.27 7.33 7.48 7.49 7.54 7.55 7.60 7.68 7.68 7.73 7.81 8.20 8.20
459.1296 317.0666 315.0870 435.1306 647.2142 451.1029 271.0608 271.0607 315.0873 317.0664 631.1474 339.1236 315.0870 227.0704 271.0975 315.0873 271.0973 315.0871
-H -H +HCOO +HCOO -H +HCOO +HCOO +HCOO +HCOO -H +HCOO -H -H -H +HCOO +HCOO
Observed CCS (Ų) 190.59 201.44 159.72 156.83 264.57 171.20 157.63 208.33 230.21 190.40 168.46 273.74 183.33 186.05 159.20 227.43
Total Fragments Found 3 0 0 0 0 0 0 6 3 0 0 0 0 1 0 1
189 833 887 482 523 1761 472 214 1928 1249 365 80
-H +HCOO -H +HCOO -H -H -H -H -H +HCOO +HCOO +HCOO
190.63 158.03 196.20 195.29 237.47 189.03 182.77 222.91 162.65 156.73 228.27 188.29
2 0 3 3 0 2 0 0 2 0 0 0
2193 84 177 3035 145 2375
-H -H -H -H -H -H
162.34 183.47 164.72 162.60 162.79 162.11
3 0 2 3 1 2
Response
Adducts
1481 230 235 236 4623 144 245 591 594 493 95 1762 86 610 400 451
8.22 8.27 8.41 8.42 8.46 8.46 8.54 8.56 8.73 8.81 8.88 8.94 8.94 9.01 9.10 9.10 9.25 9.25
Table 1: Cont’d .
Component name
178 179 180 181 182 183
Dihydroresveratrol Protosappanin A Caesalpins P Caesalpins P 3,5,4'-Trihydroxystilbene 3,7-Dihydroxy-2,4dimethoxyphenanthren e Moracin F Feroxin B 2,3,5,4'-Tetrahydroxystilbene-2-Oβ-D-glucopyranoside Thannilignan Cinchonain Ia Obovatol 1,7-Bis(4-hydroxyphenyl)hepta-4E,6E-dien-3-one 3,7-Dihydroxy-2,4dimethoxyphenanthrene 3,7-Dihydroxy-2,4dimethoxyphenanthren e (1R,2S,3R,6'R,7'R)-3, 7'-Bis(3,4dihydroxy- phenyl)1,1',2,2',3,3',4,4'-octahydro-1,1'binaphthyl-2,2',4',6,6',8-hexaol Feroxin B Feroxin B Feroxin B Feroxin B Feroxin B Caesalpins P Magnaldehyde B Moracin H
184 185 186 187 188 189 190 191 192 193
194 195 196 197 198 199 200 201
Observed m/z 229.0863 317.0665 299.0553 299.0554 273.0772 315.0871
Observed RT (min) 9.25 9.32 9.38 9.38 9.43 9.43
-H +HCOO -H -H +HCOO +HCOO
Observed CCS (Ų) 164.10 156.08 206.11 165.76 194.94 162.57
Total Fragments Found 0 0 0 0 0 0
331.0829 647.2146 405.1194
105 225 333
+HCOO -H -H
161.89 237.90 194.41
0 0 0
9.71 10.06 10.06 10.07
531 1040 104 93
-H -H +HCOO +HCOO
181.17 189.28 187.21 191.70
0 2 0 0
315.0875
10.10
280
+HCOO
163.65
0
315.0870
10.41
281
+HCOO
161.92
0
619.1833
10.77
118
+HCOO
232.41
0
647.2148 647.2150 647.2134 647.2132 647.2134 299.0560 325.1080 337.1085
10.78 11.03 11.12 11.25 11.47 11.52 11.58 11.58
353 686 1241 743 411 135 259 384
-H -H -H -H -H -H +HCOO -H
239.15 240.08 239.51 240.96 238.81 167.62 181.99 184.69
0 0 0 0 0 0 0 1
Response
Adducts
71 200 658 373 131 370
9.50 9.54 9.57
329.1390 451.1034 327.1240 339.1240
Table 1: Cont’d .
Component name
202 Moracin C 203 2,6-Bis(4-hydroxyphenyl)-3′,5dimethoxy-3-hydroxybibenzyl 204 2,7-Dihydroxy-1-(4'hydroxybenzyl)-4- methoxy9,10- dihydrophenanthrene-4'-Oglucoside 205 Protosappanin A 206 Brazilein 207 Brazilein 208 (R)-Prechrysophanol 209 Caesalpins P 210 2,3,5,4'-Tetrahydroxystilbene-2-Oβ-D-glucopyranoside 211 (R)-Prechrysophanol 212 2,7-Dihydroxy-4methoxyphenanthrene- 2-Oglucoside 213 Agrimol E 214 Erianin 215 Blestrianol C 216 Kukoamine A 217 Yakuchinone A 218 Kukoamine A 219 Terchebin 220 Yakuchinone A 221 (3R,4R)-3,4-trans-7,2′Dihydroxy-4′- methoxy-4-[(3R)2′,7-dihydroxy-4′-methoxyisoflavan-5′-yl]-isoflavan 222 Geraniin 223 Geraniin 224 Sodium ferulate
Observed m/z 355.1179 469.2035
Observed RT Response (min) 11.58 77 11.60 105
+HCOO -H
Observed CCS (Ų) 180.97 211.95
Total Fragments Found 0 0
555.1859
11.62
127
+HCOO
220.40
0
271.0617 283.0610 283.0613 257.0820 299.0564 405.1208
11.80 11.91 11.91 12.37 12.78 13.16
590 126 95 1267 812 118
-H -H -H -H -H -H
155.83 162.19 214.63 156.75 165.56 194.13
0 0 0 0 0 0
257.0811 447.1284
13.16 16.44
119 130
-H +HCOO
151.98 210.60
0 0
625.2296 317.1408 631.1972 529.3027 311.1658 529.3024 999.0961 311.1663 541.1865
16.45 16.47 16.47 16.49 16.49 16.50 16.56 16.56 16.56
89 86 113 129 169 727 2723 108 134
-H -H +HCOO -H -H -H +HCOO -H -H
245.77 174.75 235.15 292.55 186.18 227.90 244.07 186.85 227.20
1 0 1 6 0 2 95 0 1
997.0781 997.0781 215.0332
16.96 17.03 17.04
857 840 85
+HCOO +HCOO -H
226.03 308.71 139.62
1 0 0
Adducts
Table 1: Cont’d .
Component name
225 226 227 228 229 230
244 245 246 247 248 249 250 251
Kukoamine A Tellimagrandin II Renifolin Geraniin Erianin 1,2,6-Tri-O-galloyl-β-Dglucopyranoside Laevigatin A Castalagin Kukoamine A Furosin 1-O-Galloylpedun- culagin Pedunculagin_1 Casuarinin Erianin Geraniin Yakuchinone B Yakuchinone A 1,2,3,6-Tetra-O-galloyl- β-Dglucopyranoside 1,2,3,6-Tetra-O-galloyl- β-Dglucopyranoside Dendroflorin Blestritin A Meliadanoside B Cyclopseudohypericin Asebotin Erianin Blestritin A Tubuloside A
252 253 254 255
Protocatechuic aldehyde Agrimol D Tubuloside A Protocatechuic aldehyde
231 232 233 234 235 236 237 238 239 240 241 242 243
Observed m/z 529.3029 983.0995 351.1465 997.0799 363.1454 635.0893
Observed RT (min) 17.06 17.06 17.07 17.09 17.12 17.15
-H +HCOO -H +HCOO +HCOO -H
Observed CCS (Ų) 224.10 288.91 175.87 231.98 183.52 199.46
Total Fragments Found 0 0 2 28 0 2
801.0809 933.0655 529.3018 649.0683 981.0857 783.0697 981.0833 317.1387 997.0794 355.1561 357.1715 787.0998
972 1220 182 781 5150 1668 4789 183 1833 322 147 220
-H -H -H -H +HCOO -H +HCOO -H +HCOO +HCOO +HCOO -H
207.80 224.95 223.41 194.41 226.24 204.34 226.20 182.59 229.31 185.48 191.81 201.07
2 2 0 17 12 36 30 0 2 0 0 19
18.49
123
-H
185.00
26
257.0462 621.2485 327.1088 501.0634 495.1497 317.1402 621.2491 827.2623
18.49 18.49 18.50 18.50 18.50 18.51 18.51 18.51
139 181 95 88 132 165 124 93
158.75 235.42 165.68 195.93 214.78 174.44 243.41 166.83
2 0 3 0 5 2 1 15
137.0240 653.2597 827.2633 137.0240
18.52 18.55 18.56 18.56
172 90 91 180
-H +HCOO -H -H +HCOO -H +HCOO -H, +HCOO -H -H -H -H
113.46 146.16 167.20 121.59
0 0 1 0
Response
Adducts
1018 91 71 1800 125 153
17.40 17.43 17.56 17.57 17.60 17.68 17.78 17.90 18.33 18.49 18.49 18.49
787.0994
3.2 Functional group characteristics Figure 1 showed the spectrum of the C. nitida extracts containing the functional group's characteristics. The output results revealed the appearance of three categories of the functional peaks which include the broad, sharp and weaker peaks. One broad peak was identified with a wavenumber 3318 cm-1 indicating the presence of the hydroxyl group[9]. Three conspicuous sharp but medium peaks were identified with wavelengths 2984, 1600 and 882 cm-1 corresponding to C-H symmetric, C-H2, and C-H aromatic bonds, respectively[9]. Moreover, three weak peaks were identified at the wavenumbers 2888, 1380 and 1093882 cm-1 indicating
the presence of fatty acid C-H, symmetric bending and phenolic bonds, respectively. Lastly, the highest peak was observed at the wavenumber 1045 cm-1 suggesting the symmetric stretching of =C-O-C- bonds [9]. On the overall, the application of electromagnetic microwave energy disrupted and disoriented the bonding structure in the cellulosic cell wall which triggered the formation of the aforementioned new peaks.
Figure 1: FTIR spectrum of C. nitida extracts 3.3 Thermogravimetry and calorimetry elucidation Thermogravimetry analysis and differential scanning calorimetry were applied to determine the stability of C.nitida to heat. This is important since it shows a stage-by-stage heat profile of the samples. The results from the output data revealed four-staged heat profiles which include 50137.5, 137.5 -175, 175-380, 380 – 430 and > 500 °C (Figure 2). The early-stage (50-137.5 °C) of heating involved the induction and weakening of the cellulosic bonds in the plant matrix with a resultant mass loss of 4.09 mg. The second (137.5 -175°C) and third stages 175-380 °C) involves the eventual release of the secondary metabolites from the sample with a corresponding mass loss of 18.5 and 38.20 %, respectively. At the final stage, 380 – 430 °C, of the heat profile the plant matrix became deteriorated and eventually denatured at a temperature above 501°C.
Figure 2 Thermogravimetric analysis spectra of phenolic extract from dried C.nitida extract Figure 3 showed the analyzed output data obtained from DSC analysis. This was employed to support the TGA results with an onset temperature of 131.6 °C (-0.347 mW/mg). The specific heat capacity at the glass transition stage was measured at 1.744 J/g*K. The lowest peak was observed at 82.2 °C with a heat flow of -1.216 mW/mg.
Figure 3 Differential scanning calorimetry curve of dried C.nitida extract
3.4 BET-physisorption The characteristic pore diameter-to-area profile for microwave extraction processes is presented in Figure 4. The output data showed a sharp decline in the microstructural characteristics of the plant matrix. This reduction indicated textural and dispersive changes in the structure of the C.nitida as a result of the irreversible effects of the microwave electromagnetic waves [10]. This clearly revealed that microwave extraction left an irreversible transformation in the microchemical and microstructural configuration of the C.nitida pod wastes.
Figure 4 Pore diameter-to-area profile 3. Conclusion The dataset presented in this study involves the functional groups, chemical profile, thermal stability, and textural characteristics of the kola nut pod sample. The extracts were characterized via Fourier transform infrared (FTIR), Liquid chromatography-QToF Spectrometer (LCMS/QToF), Thermogravimetry analyzer (TGA), Differential scanning calorimetry (DSC), Field emission scanning electron microscopy (FESEM) and Brunauer-Emmett-Teller (BET), respectively. The result of these analyses succinctly sheds more light on the effect of microwave heating on the extraction of phenolic constituents from C.nitida. The results of the microchemical and microstructural characterization elucidated the effect of microwave extraction on the eventual release of phenolic constituents encrypted in the precursor of the cellulosic sites
References [1]
R. Sindhu, Conversion of food and kitchen waste to value-added products. J. Environ. Manage. 241 (2019) 619–630.
[2]
O. A. Olalere, H. N. Abdurahman, and C. Y. Gan, Microwave-enhanced extraction and mass spectrometry fingerprints of polyphenolic constituents in Sesamum indicum leaves. Ind. Crops Prod., 131 (2019) 151–159.
[3]
M. A. Olmedo-Suarez and M. P. Canizares-Macías, Method for the Production of natural vanilla extracts using a conventional microwave oven. Curr. Microw. Chem. 2 (2015) 24– 31.
[4]
O. A. Olalere, H. Abdurahman, R. M. Yunus, and O. R. Alara, Data article on elemental and metabolomic-based alkaloidal composition in black pepper oleoresin using a positive ESI-mode LC-QToF and ICP-mass spectroscopy. Data in Brief, (2018).
[5]
O. A. Olalere, N. H. Abdurahman, R. bin M. Yunus, O. R. Alara, and N. A. Kabbashi, Chemical fingerprinting of biologically active compounds and morphological transformation during microwave reflux extraction of black pepper. Chem. Data Collect. 17–18 (2018) 339–344.
[6]
T. S. Ballard, P. Mallikarjunan, and S. O. Keefe, Optimizing the extraction of phenolic antioxidant compounds from peanut skins. Dissertation submitted to the Faculty of Virginia Polytechnic Institute and State University, Blacksburg, VA, 2008.
[7]
M. Borucka, Identification of volatile and semi-volatile organic compounds emitted during thermal degradation and combustion of triadimenol. J. Therm. Anal. Calorim. 138 (2019) 1–14.
[8]
O. A. Olalere, H. N. Abdurahman, R. Bin, and M. Yunus, Parameters Affecting antiradical, elemental composition and microstructural elucidation in the heat reflux extraction of dried piper nigrum seedlings parameters affecting antiradical, elemental composition and microstructural elucidation. Jundishapur J. Nat. Pharm. Prod. 14 (2019) e57498.
[9]
J. K. Adesanwo, S. B. Ogundele, D. A. Akinpelu, and A. G. McDonald, Chemical Analyses, antimicrobial and antioxidant activities of extracts from Cola nitida Seed,” J. Explor. Res. Pharmacol. 2 (2017) 67–77.
[10] J. Balamaze, J. H. Muyonga, and Y. B. Byaruhanga, Physico-chemical characteristics of selected jackfruit (Artocarpus Heterophyllus Lam) varieties. J. Food Res. 8 (2019) 11-19.
Dataset on the Microstructural and Microchemical Characterization of Valorized Cola nitida Pod Wastes Olalere Olusegun Abayomi , Chee-Yuen Gan , Abdurahman Hamid Nour , Muhammad Sheraz Ahmad , Aziz Qannaf Zaid , Omar Abed Habeeb PII: DOI: Reference:
S2405-8300(20)30067-7 https://doi.org/10.1016/j.cdc.2020.100356 CDC 100356
To appear in:
Chemical Data Collections
Received date: Revised date: Accepted date:
17 October 2019 28 January 2020 13 February 2020
Please cite this article as: Olalere Olusegun Abayomi , Chee-Yuen Gan , Abdurahman Hamid Nour , Muhammad Sheraz Ahmad , Aziz Qannaf Zaid , Omar Abed Habeeb , Dataset on the Microstructural and Microchemical Characterization of Valorized Cola nitida Pod Wastes, Chemical Data Collections (2020), doi: https://doi.org/10.1016/j.cdc.2020.100356
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Dataset on the Microstructural and Microchemical Characterization of Valorized Cola nitida Pod Wastes Olalere Olusegun Abayomi1*, Chee-Yuen Gan1*, Abdurahman Hamid Nour2, Muhammad Sheraz Ahmad 2, Aziz Qannaf Zaid2, Omar Abed Habeeb2 1
Analytical Biochemistry Research Center (ABrC), Universiti Sains Malaysia (USM), 11800 Gelugor, Penang, Malaysia 2
Chemical and Process Engineering. Universiti Malaysia Pahang (UMP), 26300, Gambang, Malaysia Corresponding author: [email protected] (Gan C.Y.) ; [email protected] (Olalere O.A.) Abstract The inherent environmental effects of the accumulated kola nut pod waste products have become a subject of discussion among many researchers. The need then arises for their alternative use as nutraceutical bioproducts. The physical and chemical analytical techniques are often required for the standardization of these bioproducts in order to determine and maintain their quality characteristics. The dataset presented in this study provided information on the chemical profile, physisorption and thermo-analytical screening of Cola nut pod extracts. Six sets of physicochemical methods were employed to characterize the phenolic extracts. The result obtained clearly revealed the presence of two-hundred and fifty-five phenolic bioactive. Also presented was the thermal stability, morphological and microstructural surface area configuration of the Cola nitida pod extracts. The information obtained from this study could be used in determining the quality of food wastes bioproducts in nutria-pharmaceutical applications. Keywords: Brunauer-Emmett-Teller (BET), Cola nitida; Differential scanning calorimetry (DSC), Thermogravimetry analysis (TGA)
Specification Table Subject area More specific subject area Type of data How data was acquired
Microchemical science Food characterization Table, Figure, Spectra a) The dataset was acquired for both positive and negative ESI-mode using LC-MS/QToF (Waters, USA). b) Thermo-analytical elucidation using TGA (Model Q500-V6.4, Germany) and DSC scanning calorimeter (model-NETZSCH DSC 214) c) Surface area elucidation using BrunauerEmmett-Teller (BET)
Data accessibility
d) Functional group characteristics using the Thermo-Nicolet spectrometer (iS5 iD7-ATR, Germany). The dataset consisting of tables, spectra, and figures can be found along with the article
1. Rationale The inherent hazard of agricultural wastes to the environment necessitates their conversion to useful-bioproducts [1]. The polyphenolic constituents of kola nut pod are widely applied in food, biopharmaceutical, and petrochemical industries. The need then arises for a physicochemical analysis that will ensure and monitor the nutritional and medicinal quality of the bioproducts from physical and chemical degradation [2]. The dataset presented a succinct microstructural, microchemical and thermophysical characterization of C.nitida pod extracts. The data consists of the phenolic profiles (Table 1) of the C.nitida oleoresin extracts obtained from the Liquid chromatography-QToF Spectrometer (LC-MS/QToF). The dried extracts were characterized to determine the effect of electromagnetic waves from microwave extractor on the thermal stability, functional group characteristics, morphological features and microstructural surface area using Thermogravimetry analyzer (TGA), Differential scanning calorimetry (DSC), Fourier transform infrared (FTIR), Field emission scanning electron microscopy (FESEM) and Brunauer-Emmett-Teller (BET). 2. Procedure 2.1 Raw material preparation The kola nut pods wastes were harvested, air-dried, crushed and sieved into particle size (< 0.50 mm) using a set of standard sieves. The extract was prepared using the microwave extractor (Ethos Milestone, USA) operated in a three-level temperature setting. The first set involves the use of moderate heat (40 °C) to trigger off the induction process which helps in breaking up the cellulosic cell wall of the sample. The second setting involves the extraction temperature (60 °C), while the last stage involves the cooling stage. The C. nitida was loaded into the microwave reactor and the bioproduct was extracted at the microwave power of 450 W, the irradiation time of 5 min, using 60 % ethanol as extracting solvent [3]. After extraction, the resulting bioproduct was unloaded from the microwave reactor and filtered using a vacuum pump (VP250N, Zhejiang, China). The filtrate was thereafter evaporated at 78 °C under vacuum to obtain a semisolid oleoresin extract, which was later subjected to spray-drying and refrigerated for further microchemical characterization and surface probes. 2.2 LC-MS chemical profiling The C. nitida oleoresin extracts were analyzed using Vion Ion Mobility QTOF MS, Waters, (USA) with the aid of an ACQUITY UPLCHSS-T3 column 2.1 x 100 mm and particle size 1.8 mm). The extract was pre-treated and the concentration adjusted to 20 ppm before injection into the LC–MSQ- the time of flight mass spectrometer according to the method employed by Olalere et al., [4]. The peak of parent and daughter fragmentation of different components was identified using a negative electron-spray ionization mode [5].
2.3 Fourier transformed infrared spectroscopy (FT-IR) The Fourier Transform Infrared (FTIR) spectroscopic analysis was conducted according to Olalere et al., [6].The functional group characteristics of the dried C. nitida powder was determined using a Thermo-Nicolet spectrometer (iS5 iD7-ATR, Germany). The spectra interpretation was performed with the aid of a Thermoscienctific OMNIC software (Vs. 9.0). The minimum and maximum range of the wavenumber was 500 cm-1 and 4000 cm-1. 2.4 Thermogravimetry analysis (TG) and Differential Scanning Calorimetry (DSC) The TGA curves were generated using an integrated TG-DTA assemblage (Model Q500-V6.4, Germany). The extracts (5.994 mg) were subjected to a temperature range between 30 and 500 °C inside an alumina pan of under atmospheric nitrogen (N2) at a heating rate of 10 °C min-1 and gas flow rate of 20 mL min-1[7]. Moreover, the DSC curves of the C. nitida pod extracts were generated using a thermogravimetric calorimeter (NETZSCH DSC-214 model). The sample mass (5.0 mg) was subjected to atmospheric nitrogen at the flow rate range 40 – 60 mL min -1. The thermal stability test was conducted at a temperature ranging from 25 – 550 °C with a heating rate of 10 K min-1. Moreover, pure indium (m. p. 156 °C) was employed to calibrate the calorimetry analyzer at the standard experimental condition. 2.5 Brunauer-Emmett-Teller (BET) In this study, the BET surface area, pore-volume, and pore size of the C. nitida were measured by nitrogen physisorption at N2 liquefaction temperature of 77 K on a Surfer Thermo Scientific unit. The textural properties of the samples were measured using an accurately weighed 0.5 g of the C. nitida [8]. This was followed by the adsorption/desorption stage involving the degassing of samples in slow mode at 423 K for 3 h. Fast mode degassing was thereafter initiated at 573 K for 12 h to remove the inherent moisture in the sample. The sample was then analyzed in a Dewar flask filled with liquid N2 for physisorption evaluation. The information obtained from the microstructure was analyzed with the aid of a Surfer Acquisition computer software connected to the instrument. 3. Data, value, and validation 3.1 Identification of phenolic content The functional phenolic secondary metabolites in C.nitida were tentatively identified and quantified using mass spectrometry techniques. The results obtained identified a total of 255 phenolic constituents with the major bioactive compounds such as Tribulusamide B (m/z =683.2261) and Cearoin (m/z =289.07). The identified and quantified secondary metabolites are partly responsible for the nutritional and medicinal potential of the valorized C. nitida pod. Table 1 is the output file from LCMS-QToF spectrometer containing the summary of all bioactive phenolic compounds identified with their mass-to-charge ratio, fragmented ions and respective retention time. Table 1: Tentative Phenolic compounds identified in the C. nitida extracts by LCMS-Q-TOF .
Component name
1
DO 19
Observed m/z 585.1785
Observed RT (min) 0.39
Observed CCS (Ų) +HCOO 212.47
Response Adducts 100
Total Fragments Found 1
2
Tribulusamide B
683.2261
0.39
316
+HCOO 184.61
0
3
Tribulusamide B
683.2261
0.39
766
+HCOO 320.24
4
4
Tribulusamide B
683.2261
0.40
6857
+HCOO 266.22
7
5
Tribulusamide B
683.2261
0.40
21588
+HCOO 224.91
6
6
2,3,5,4'Tetrahydroxystilbene-2O-β-Dglucopyranoside Haematoxylin Dihydrooxyresveratrol Euparin Piceatannol Protosappanin C Methyl-5-Ocaffeoylquinate 2,4,6Trihydroxyacetophenon e-2,4-di-O-β-Dglucopyranoside Moracin M Moracin M-3′-O-βD- glucopyranoside p-Tolualdehyde
451.1258
0.40
145
+HCOO 187.47
1
301.0723 245.0822 215.0718 289.0720 301.0721 367.1052
0.40 0.41 0.41 0.41 0.42 0.42
85 912 101 6161 335 934
-H -H -H +HCOO -H -H
238.28 152.49 156.75 152.91 156.30 170.83
0 0 2 0 1 2
491.1404
0.42
221
-H
203.81
0
287.0564 449.1102
0.43 0.44
354 204
+HCOO 157.26 +HCOO 187.21
0 0
167.0353
0.44
167
+HCOO 123.08
0
7 8 9 10 11 12 13
14 15 16
Table 1: Cont’d .
Component name
17
Protocatechuic aldehyde
18 19 20 21 22 23
Sodium ferulate Procyanidin C-1 Dihydrooxyresveratrol Piceatannol p-Tolualdehyde Moracin M-3′-O-β-Dglucopyranoside Koaburaside Piceatannol Vanillin 2,3,5,4'-Tetrahydroxystilbene-2O-β-D-glucopyranoside Protocatechuic aldehyde Protocatechuic aldehyde Protocatechuic aldehyde 2,3,5,4'-Tetrahydroxystilbene-2O-β-D-glucopyranoside
24 25 26 27 28 29 30 31
Observed m/z 137.0242
Observed RT (min) 0.46
-H
Observed CCS (Ų) 122.79
Total Fragments Found 0
215.0326 911.2030 245.0825 289.0717 167.0346 449.1091
352 144 327 3034 218 420
-H +HCOO -H +HCOO +HCOO +HCOO
171.45 268.49 153.74 153.23 124.26 190.69
0 0 0 0 0 0
2.45 2.54 2.70 2.96
117 4633 135 391
-H +HCOO +HCOO +HCOO
168.45 153.51 185.22 189.10
1 0 0 0
3.08 3.16 3.18 3.37
1476 1783 760 334
-H -H -H +HCOO
124.98 120.03 140.94 207.35
0 0 0 0
Response
Adducts
198
0.48 1.96 2.03 2.06 2.07 2.31
331.1028 289.0719 197.0450 451.1241 137.0242 137.0242 137.0242 451.1255
32 33
2,4,6-Trihydroxyacetophenon e-2,4di-O-β-D-glucopyranoside 4-Hydroxyacetophenone
491.1417
3.42
451
-H
206.25
1
135.0448
3.46
1911
-H
130.34
0
Observed m/z 451.1250
Observed RT (min) 3.53
Response
Adducts
337
+HCOO
Observed CCS (Ų) 189.60
Total Fragments Found 0
363.1440 491.1401
3.55 3.63
189 231
+HCOO -H
174.88 205.41
0 0
287.0556 451.1022 451.1240
3.72 3.73 3.75
401 415 362
+HCOO -H +HCOO
223.56 217.75 188.93
0 14 0
451.1247
3.82
1001
+HCOO
187.82
0
401.1434 151.0393 245.0452
3.84 3.89 3.90
88 126 205
+HCOO -H -H
195.16 159.80 165.91
0 0 1
287.0560 271.0611 121.0291 221.0818
3.90 3.91 3.91 3.91
484 259 227 335
+HCOO -H -H -H
199.28 155.97 126.96 144.35
1 10 0 0
287.0561 303.0496 137.0240 289.0718
3.91 3.91 3.91 3.91
719 159 323 29671
225.10 157.95 184.83 153.63
0 2 1 7
245.0818 137.0240
3.92 3.92
5375 440
+HCOO +HCOO -H +HCOO, -H -H -H
152.58 163.62
1 1
Table 1: Cont’d .
Component name
34
48 49 50 51
2,3,5,4'Tetrahydroxystilbene-2O-β-D-glucopyranoside Erianin 2,4,6Trihydroxyacetophenon e-2,4-di-O-β-Dglucopyranoside Moracin M Cinchonain Ia 2,3,5,4'Tetrahydroxystilbene-2O-β-D-glucopyranoside 2,3,5,4'Tetrahydroxystilbene-2O-β-Dglucopyranoside Feroxin A Vanillin 2,4,4′,6′-Tetrahydroxybenzophenone Nobilone Protosappanin A p-Tolualdehyde 4-(4'-Hydroxy-3',5'dimethoxyphenyl)3- buten-2-one Moracin M Dendroflorin Protocatechuic aldehyde Cearoin
52 53
Dihydrooxyresveratrol Sesamol
35 36
37 38 39
40
41 42 43 44 45 46 47
Table 1: Cont’d
.
Component name
54 55 56
Cearoin Pyrogallic acid Nobilone
57
2,4,6-Trihydroxyacetophenon e2,4-di-O-β-D glucopyranoside Dendroflorin 2,3,5,4'-Tetrahydroxystilbene-2O-β-D-glucopyranoside Procyanidin C-1 2,3,5,4'-Tetrahydroxystilbene-2O-β-D-glucopyranoside Cinchonain Ia Moracin F Procyanidin C-1 Brazilein Cinchonain Ia Apocynin B Nobilone 1,2,6-Tri-O-galloyl-β-Dglucopyranoside Cinchonain Ia Procyanidin C-1 2,3,5,4'-Tetrahydroxystilbene-2O-β-D-glucopyranoside Feroxin A Protocatechuic aldehyde 4-(4'-Hydroxy-3',5'dimethoxyphenyl)-3buten-2-one Sesamol Cearoin Cearoin
58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 74 75
76 77 78
Observed m/z 289.0717 125.0242 287.0561
Observed RT (min) 3.92 3.92 3.92
Response
Adducts
2498 316 2846
+HCOO -H +HCOO, -H
Observed CCS (Ų) 222.06 163.23 159.45
491.1418
Total Fragments Found 1 0 2
4.12
417
-H
207.51
0
303.0510 451.1253
4.12 4.22
231 369
+HCOO +HCOO
187.94 185.79
0 0
865.1979 451.1258
4.38 4.41
3502 379
-H +HCOO
270.11 206.88
1 0
451.1024 331.0828 865.1976 329.0678 451.1025 467.0978 287.0553 635.0884
4.50 4.51 4.52 4.53 4.54 4.76 4.82 4.83
425 102 2172 245 692 127 347 133
-H +HCOO -H +HCOO -H -H +HCOO -H
188.17 166.52 266.40 176.24 217.84 230.34 221.55 231.48
3 1 0 0 4 1 1 0
451.1033 865.1975 451.1243
4.83 5.04 5.07
505 1674 2245
-H -H +HCOO
218.99 269.08 188.10
18 1 0
401.1444 137.0241 221.0822
5.13 5.15 5.17
279 274 345
+HCOO -H -H
195.88 124.45 144.80
2 0 0
137.0241 289.0715 289.0715
5.17 5.17 5.17
827 35074 2568
-H +HCOO, -H +HCOO
164.76 153.69 197.56
1 7 2
Table 1: Cont’d .
Component name
79 80 81 82 83 84 85 86
Dihydrooxyresveratrol Dihydrooxyresveratrol Nobilone Moracin M Vanillin Cearoin Pyrogallic acid Dendroflorin
87 88
Protosappanin A 2,4,4′,6′-Tetrahydroxybenzophenone Aspidinol Feroxin A Cinchonain Ia Procyanidin C-1 Caesalpins P Brazilein Protosappanin E-1 2,7-Dihydroxy-1,3-di(phydroxybenzyl)-4methoxy-9,10dihydrophenanthrene Terrestriamide Protosappanin E-1 p-Tolualdehyde Piceatannol Protosappanin A Terrestriamide Apocynin B Procyanidin C-1 Moracin M-3′-O-β-Dglucopyranoside Procyanidin C-1 4-Hydroxyacetophenone Feralolide Moracin F Hematine
89 90 91 92 93 94 95 96
97 98 99 100 101 102 103 104 105 106 107 108 109 110
Observed m/z 245.0818 245.0818 287.0554 287.0554 151.0395 289.0715 125.0242 257.0447
Observed RT (min) 5.17 5.18 5.18 5.18 5.18 5.18 5.18 5.18
-H -H +HCOO, -H +HCOO -H +HCOO -H -H,+HCOO
Observed CCS (Ų) 152.52 217.74 158.90 223.79 160.27 221.67 163.26 154.80
Total Fragments Found 1 0 2 0 0 3 0 4
271.0601 245.0447
236 201
-H -H
156.97 151.08
8 1
5.31 5.31 5.51 5.52 5.53 5.53 5.53 5.54
300 820 439 1437 73 202 233 243
+HCOO +HCOO -H -H -H +HCOO +HCOO -H
197.72 196.48 189.84 262.93 228.75 161.99 239.16 200.07
0 1 1 0 3 0 0 0
372.1090 631.1450 167.0344 289.0712 271.0608 372.1079 467.0996 865.1982 449.1087
5.55 5.59 5.62 5.68 5.69 5.70 5.74 5.74 5.89
291 235 397 1523 210 151 171 3253 8343
+HCOO +HCOO +HCOO +HCOO -H +HCOO -H -H +HCOO
172.33 223.47 126.82 221.38 216.48 170.68 240.19 270.81 190.93
0 1 0 0 0 0 0 1 1
865.1979 135.0446 343.0833 331.0812 299.0547
5.91 5.98 6.11 6.12 6.14
9530 236 219 251 415
-H -H -H +HCOO -H
271.03 129.83 181.27 167.12 164.31
11 0 0 3 2
Response
Adducts
5577 187 3485 1028 126 3935 461 142
5.18 5.18
269.1025 401.1449 451.1037 865.1980 299.0551 329.0659 631.1449 453.1723
Table 1: Cont’d .
Component name
111 112 113 114 115 116 117 118 119 120 121 122 123 124 125 126 127 128 129 130 131 132 133 134 135 136 137 138
Protosappanin C Protosappanin C (R)-Prechrysophanol Protosappanin C Phenol Protosappanin C 3,5,4'-Trihydroxystilbene Euparin Moracin M Caesalpins J Terrestriamide Procyanidin C-1 Apocynin B Terrestriamide Polydatin 3,5,4'-Trihydroxystilbene 3,5,4'-Trihydroxystilbene Polydatin Confusarin Smilaxin Piceatannol Procyanidin C-1 Phenol Protosappanin C Protosappanin C Euparin (R)-Prechrysophanol 7,2′,3′-Trihydroxy-4′methoxy-isoflavan Protosappanin C Caesalpins P Moracin F Blestritin B Brazilein
139 140 141 142 143
Observed m/z 301.0715 301.0714 257.0815 301.0714 139.0401 301.0715 273.0755 215.0713 287.0555 315.0868 372.1094 865.1982 467.0984 372.1087 435.1314 227.0709 227.0709 389.1253 345.0977 315.0868 289.0713 865.1996 139.0396 301.0719 301.0719 215.0713 257.0823 333.0969
Observed RT (min) 6.14 6.14 6.14 6.15 6.15 6.15 6.15 6.15 6.15 6.16 6.34 6.41 6.61 6.79 6.80 6.87 6.88 6.88 6.89 7.01 7.07 7.11 7.13 7.13 7.14 7.14 7.14 7.14
301.0718 299.0556 331.0821 531.2036 329.0666
7.15 7.15 7.15 7.16 7.16
-H -H -H -H +HCOO -H +HCOO -H +HCOO -H +HCOO -H -H +HCOO +HCOO -H -H -H +HCOO -H +HCOO -H +HCOO -H -H -H -H +HCOO
Observed CCS (Ų) 241.22 210.56 156.74 186.62 164.10 155.85 158.67 158.04 223.73 170.08 173.62 275.25 194.57 171.49 198.63 206.92 153.74 203.77 168.22 160.42 224.43 267.65 163.37 202.73 155.80 158.10 156.15 242.44
Total Fragments Found 1 1 2 1 0 6 0 2 0 3 0 1 1 0 0 0 0 1 0 0 0 1 0 1 7 2 3 0
-H -H +HCOO +HCOO +HCOO
240.75 164.68 169.34 221.98 166.69
1 1 1 0 0
Response
Adducts
309 261 664 413 127 4818 164 1430 412 569 337 1153 147 449 166 117 95 86 117 742 1476 1261 159 514 5942 1727 846 100 396 807 560 98 344
Table 1: Cont’d .
Component name
144 145 146 147 148 149 150 151 152 153 154 155 156 157 158 159
Cinchonain Ia Protosappanin A Haematoxylin Protosappanin A Procyanidin C-1 Confusarin Protosappanin A Protosappanin E-1 Protosappanin E-1 Cinchonain Ia Smilaxin Procyanidin C-1 Thannilignan Cinchonain Ia Moracin M 3,7-Dihydroxy-2,4dimethoxyphenanthren e-3-Oglucoside Kuzubutenolide A Protosappanin A Caesalpins J Polydatin Feroxin B Cinchonain Ia Protosappanin A Protosappanin A Caesalpins J Protosappanin A Protosappanin E-1 1,7-Bis(4-hydroxyphenyl)hepta-4E,6E-dien-3-one Smilaxin 3,5,4'-Trihydroxystilbene (-)-Vestitol Caesalpins J (-)-Vestitol Caesalpins J
160 161 162 163 164 165 166 167 168 169 170 171 172 173 174 175 176 177
Observed m/z 451.1036 271.0606 347.0773 317.0661 865.1982 345.0989 317.0666 631.1453 631.1454 451.1039 361.0933 865.1977 329.1407 451.1038 287.0560 477.1413
Observed RT (min) 7.21 7.22 7.26 7.27 7.33 7.48 7.49 7.54 7.55 7.60 7.68 7.68 7.73 7.81 8.20 8.20
459.1296 317.0666 315.0870 435.1306 647.2142 451.1029 271.0608 271.0607 315.0873 317.0664 631.1474 339.1236 315.0870 227.0704 271.0975 315.0873 271.0973 315.0871
-H -H +HCOO +HCOO -H +HCOO +HCOO +HCOO +HCOO -H +HCOO -H -H -H +HCOO +HCOO
Observed CCS (Ų) 190.59 201.44 159.72 156.83 264.57 171.20 157.63 208.33 230.21 190.40 168.46 273.74 183.33 186.05 159.20 227.43
Total Fragments Found 3 0 0 0 0 0 0 6 3 0 0 0 0 1 0 1
189 833 887 482 523 1761 472 214 1928 1249 365 80
-H +HCOO -H +HCOO -H -H -H -H -H +HCOO +HCOO +HCOO
190.63 158.03 196.20 195.29 237.47 189.03 182.77 222.91 162.65 156.73 228.27 188.29
2 0 3 3 0 2 0 0 2 0 0 0
2193 84 177 3035 145 2375
-H -H -H -H -H -H
162.34 183.47 164.72 162.60 162.79 162.11
3 0 2 3 1 2
Response
Adducts
1481 230 235 236 4623 144 245 591 594 493 95 1762 86 610 400 451
8.22 8.27 8.41 8.42 8.46 8.46 8.54 8.56 8.73 8.81 8.88 8.94 8.94 9.01 9.10 9.10 9.25 9.25
Table 1: Cont’d .
Component name
178 179 180 181 182 183
Dihydroresveratrol Protosappanin A Caesalpins P Caesalpins P 3,5,4'-Trihydroxystilbene 3,7-Dihydroxy-2,4dimethoxyphenanthren e Moracin F Feroxin B 2,3,5,4'-Tetrahydroxystilbene-2-Oβ-D-glucopyranoside Thannilignan Cinchonain Ia Obovatol 1,7-Bis(4-hydroxyphenyl)hepta-4E,6E-dien-3-one 3,7-Dihydroxy-2,4dimethoxyphenanthrene 3,7-Dihydroxy-2,4dimethoxyphenanthren e (1R,2S,3R,6'R,7'R)-3, 7'-Bis(3,4dihydroxy- phenyl)1,1',2,2',3,3',4,4'-octahydro-1,1'binaphthyl-2,2',4',6,6',8-hexaol Feroxin B Feroxin B Feroxin B Feroxin B Feroxin B Caesalpins P Magnaldehyde B Moracin H
184 185 186 187 188 189 190 191 192 193
194 195 196 197 198 199 200 201
Observed m/z 229.0863 317.0665 299.0553 299.0554 273.0772 315.0871
Observed RT (min) 9.25 9.32 9.38 9.38 9.43 9.43
-H +HCOO -H -H +HCOO +HCOO
Observed CCS (Ų) 164.10 156.08 206.11 165.76 194.94 162.57
Total Fragments Found 0 0 0 0 0 0
331.0829 647.2146 405.1194
105 225 333
+HCOO -H -H
161.89 237.90 194.41
0 0 0
9.71 10.06 10.06 10.07
531 1040 104 93
-H -H +HCOO +HCOO
181.17 189.28 187.21 191.70
0 2 0 0
315.0875
10.10
280
+HCOO
163.65
0
315.0870
10.41
281
+HCOO
161.92
0
619.1833
10.77
118
+HCOO
232.41
0
647.2148 647.2150 647.2134 647.2132 647.2134 299.0560 325.1080 337.1085
10.78 11.03 11.12 11.25 11.47 11.52 11.58 11.58
353 686 1241 743 411 135 259 384
-H -H -H -H -H -H +HCOO -H
239.15 240.08 239.51 240.96 238.81 167.62 181.99 184.69
0 0 0 0 0 0 0 1
Response
Adducts
71 200 658 373 131 370
9.50 9.54 9.57
329.1390 451.1034 327.1240 339.1240
Table 1: Cont’d .
Component name
202 Moracin C 203 2,6-Bis(4-hydroxyphenyl)-3′,5dimethoxy-3-hydroxybibenzyl 204 2,7-Dihydroxy-1-(4'hydroxybenzyl)-4- methoxy9,10- dihydrophenanthrene-4'-Oglucoside 205 Protosappanin A 206 Brazilein 207 Brazilein 208 (R)-Prechrysophanol 209 Caesalpins P 210 2,3,5,4'-Tetrahydroxystilbene-2-Oβ-D-glucopyranoside 211 (R)-Prechrysophanol 212 2,7-Dihydroxy-4methoxyphenanthrene- 2-Oglucoside 213 Agrimol E 214 Erianin 215 Blestrianol C 216 Kukoamine A 217 Yakuchinone A 218 Kukoamine A 219 Terchebin 220 Yakuchinone A 221 (3R,4R)-3,4-trans-7,2′Dihydroxy-4′- methoxy-4-[(3R)2′,7-dihydroxy-4′-methoxyisoflavan-5′-yl]-isoflavan 222 Geraniin 223 Geraniin 224 Sodium ferulate
Observed m/z 355.1179 469.2035
Observed RT Response (min) 11.58 77 11.60 105
+HCOO -H
Observed CCS (Ų) 180.97 211.95
Total Fragments Found 0 0
555.1859
11.62
127
+HCOO
220.40
0
271.0617 283.0610 283.0613 257.0820 299.0564 405.1208
11.80 11.91 11.91 12.37 12.78 13.16
590 126 95 1267 812 118
-H -H -H -H -H -H
155.83 162.19 214.63 156.75 165.56 194.13
0 0 0 0 0 0
257.0811 447.1284
13.16 16.44
119 130
-H +HCOO
151.98 210.60
0 0
625.2296 317.1408 631.1972 529.3027 311.1658 529.3024 999.0961 311.1663 541.1865
16.45 16.47 16.47 16.49 16.49 16.50 16.56 16.56 16.56
89 86 113 129 169 727 2723 108 134
-H -H +HCOO -H -H -H +HCOO -H -H
245.77 174.75 235.15 292.55 186.18 227.90 244.07 186.85 227.20
1 0 1 6 0 2 95 0 1
997.0781 997.0781 215.0332
16.96 17.03 17.04
857 840 85
+HCOO +HCOO -H
226.03 308.71 139.62
1 0 0
Adducts
Table 1: Cont’d .
Component name
225 226 227 228 229 230
244 245 246 247 248 249 250 251
Kukoamine A Tellimagrandin II Renifolin Geraniin Erianin 1,2,6-Tri-O-galloyl-β-Dglucopyranoside Laevigatin A Castalagin Kukoamine A Furosin 1-O-Galloylpedun- culagin Pedunculagin_1 Casuarinin Erianin Geraniin Yakuchinone B Yakuchinone A 1,2,3,6-Tetra-O-galloyl- β-Dglucopyranoside 1,2,3,6-Tetra-O-galloyl- β-Dglucopyranoside Dendroflorin Blestritin A Meliadanoside B Cyclopseudohypericin Asebotin Erianin Blestritin A Tubuloside A
252 253 254 255
Protocatechuic aldehyde Agrimol D Tubuloside A Protocatechuic aldehyde
231 232 233 234 235 236 237 238 239 240 241 242 243
Observed m/z 529.3029 983.0995 351.1465 997.0799 363.1454 635.0893
Observed RT (min) 17.06 17.06 17.07 17.09 17.12 17.15
-H +HCOO -H +HCOO +HCOO -H
Observed CCS (Ų) 224.10 288.91 175.87 231.98 183.52 199.46
Total Fragments Found 0 0 2 28 0 2
801.0809 933.0655 529.3018 649.0683 981.0857 783.0697 981.0833 317.1387 997.0794 355.1561 357.1715 787.0998
972 1220 182 781 5150 1668 4789 183 1833 322 147 220
-H -H -H -H +HCOO -H +HCOO -H +HCOO +HCOO +HCOO -H
207.80 224.95 223.41 194.41 226.24 204.34 226.20 182.59 229.31 185.48 191.81 201.07
2 2 0 17 12 36 30 0 2 0 0 19
18.49
123
-H
185.00
26
257.0462 621.2485 327.1088 501.0634 495.1497 317.1402 621.2491 827.2623
18.49 18.49 18.50 18.50 18.50 18.51 18.51 18.51
139 181 95 88 132 165 124 93
158.75 235.42 165.68 195.93 214.78 174.44 243.41 166.83
2 0 3 0 5 2 1 15
137.0240 653.2597 827.2633 137.0240
18.52 18.55 18.56 18.56
172 90 91 180
-H +HCOO -H -H +HCOO -H +HCOO -H, +HCOO -H -H -H -H
113.46 146.16 167.20 121.59
0 0 1 0
Response
Adducts
1018 91 71 1800 125 153
17.40 17.43 17.56 17.57 17.60 17.68 17.78 17.90 18.33 18.49 18.49 18.49
787.0994
3.2 Functional group characteristics Figure 1 showed the spectrum of the C. nitida extracts containing the functional group's characteristics. The output results revealed the appearance of three categories of the functional peaks which include the broad, sharp and weaker peaks. One broad peak was identified with a wavenumber 3318 cm-1 indicating the presence of the hydroxyl group[9]. Three conspicuous sharp but medium peaks were identified with wavelengths 2984, 1600 and 882 cm-1 corresponding to C-H symmetric, C-H2, and C-H aromatic bonds, respectively[9]. Moreover, three weak peaks were identified at the wavenumbers 2888, 1380 and 1093882 cm-1 indicating
the presence of fatty acid C-H, symmetric bending and phenolic bonds, respectively. Lastly, the highest peak was observed at the wavenumber 1045 cm-1 suggesting the symmetric stretching of =C-O-C- bonds [9]. On the overall, the application of electromagnetic microwave energy disrupted and disoriented the bonding structure in the cellulosic cell wall which triggered the formation of the aforementioned new peaks.
Figure 1: FTIR spectrum of C. nitida extracts 3.3 Thermogravimetry and calorimetry elucidation Thermogravimetry analysis and differential scanning calorimetry were applied to determine the stability of C.nitida to heat. This is important since it shows a stage-by-stage heat profile of the samples. The results from the output data revealed four-staged heat profiles which include 50137.5, 137.5 -175, 175-380, 380 – 430 and > 500 °C (Figure 2). The early-stage (50-137.5 °C) of heating involved the induction and weakening of the cellulosic bonds in the plant matrix with a resultant mass loss of 4.09 mg. The second (137.5 -175°C) and third stages 175-380 °C) involves the eventual release of the secondary metabolites from the sample with a corresponding mass loss of 18.5 and 38.20 %, respectively. At the final stage, 380 – 430 °C, of the heat profile the plant matrix became deteriorated and eventually denatured at a temperature above 501°C.
Figure 2 Thermogravimetric analysis spectra of phenolic extract from dried C.nitida extract Figure 3 showed the analyzed output data obtained from DSC analysis. This was employed to support the TGA results with an onset temperature of 131.6 °C (-0.347 mW/mg). The specific heat capacity at the glass transition stage was measured at 1.744 J/g*K. The lowest peak was observed at 82.2 °C with a heat flow of -1.216 mW/mg.
Figure 3 Differential scanning calorimetry curve of dried C.nitida extract
3.4 BET-physisorption The characteristic pore diameter-to-area profile for microwave extraction processes is presented in Figure 4. The output data showed a sharp decline in the microstructural characteristics of the plant matrix. This reduction indicated textural and dispersive changes in the structure of the C.nitida as a result of the irreversible effects of the microwave electromagnetic waves [10]. This clearly revealed that microwave extraction left an irreversible transformation in the microchemical and microstructural configuration of the C.nitida pod wastes.
Figure 4 Pore diameter-to-area profile 3. Conclusion The dataset presented in this study involves the functional groups, chemical profile, thermal stability, and textural characteristics of the kola nut pod sample. The extracts were characterized via Fourier transform infrared (FTIR), Liquid chromatography-QToF Spectrometer (LCMS/QToF), Thermogravimetry analyzer (TGA), Differential scanning calorimetry (DSC), Field emission scanning electron microscopy (FESEM) and Brunauer-Emmett-Teller (BET), respectively. The result of these analyses succinctly sheds more light on the effect of microwave heating on the extraction of phenolic constituents from C.nitida. The results of the microchemical and microstructural characterization elucidated the effect of microwave extraction on the eventual release of phenolic constituents encrypted in the precursor of the cellulosic sites
References [1]
R. Sindhu, Conversion of food and kitchen waste to value-added products. J. Environ. Manage. 241 (2019) 619–630.
[2]
O. A. Olalere, H. N. Abdurahman, and C. Y. Gan, Microwave-enhanced extraction and mass spectrometry fingerprints of polyphenolic constituents in Sesamum indicum leaves. Ind. Crops Prod., 131 (2019) 151–159.
[3]
M. A. Olmedo-Suarez and M. P. Canizares-Macías, Method for the Production of natural vanilla extracts using a conventional microwave oven. Curr. Microw. Chem. 2 (2015) 24– 31.
[4]
O. A. Olalere, H. Abdurahman, R. M. Yunus, and O. R. Alara, Data article on elemental and metabolomic-based alkaloidal composition in black pepper oleoresin using a positive ESI-mode LC-QToF and ICP-mass spectroscopy. Data in Brief, (2018).
[5]
O. A. Olalere, N. H. Abdurahman, R. bin M. Yunus, O. R. Alara, and N. A. Kabbashi, Chemical fingerprinting of biologically active compounds and morphological transformation during microwave reflux extraction of black pepper. Chem. Data Collect. 17–18 (2018) 339–344.
[6]
T. S. Ballard, P. Mallikarjunan, and S. O. Keefe, Optimizing the extraction of phenolic antioxidant compounds from peanut skins. Dissertation submitted to the Faculty of Virginia Polytechnic Institute and State University, Blacksburg, VA, 2008.
[7]
M. Borucka, Identification of volatile and semi-volatile organic compounds emitted during thermal degradation and combustion of triadimenol. J. Therm. Anal. Calorim. 138 (2019) 1–14.
[8]
O. A. Olalere, H. N. Abdurahman, R. Bin, and M. Yunus, Parameters Affecting antiradical, elemental composition and microstructural elucidation in the heat reflux extraction of dried piper nigrum seedlings parameters affecting antiradical, elemental composition and microstructural elucidation. Jundishapur J. Nat. Pharm. Prod. 14 (2019) e57498.
[9]
J. K. Adesanwo, S. B. Ogundele, D. A. Akinpelu, and A. G. McDonald, Chemical Analyses, antimicrobial and antioxidant activities of extracts from Cola nitida Seed,” J. Explor. Res. Pharmacol. 2 (2017) 67–77.
[10] J. Balamaze, J. H. Muyonga, and Y. B. Byaruhanga, Physico-chemical characteristics of selected jackfruit (Artocarpus Heterophyllus Lam) varieties. J. Food Res. 8 (2019) 11-19.