Effect of Different Drying Methods on the Nutritional Value of Hibiscus sabdariffa Calyces as Revealed by NMR Metabolomics
Abstract
:1. Introduction
2. Results and Discussion
2.1. Proximate Analysis
2.2. Assignment of Resonance Signals of the Metabolites
2.3. Principal Component Analysis (PCA)
2.4. Quantification of Metabolites
2.4.1. Hibiscus Acid
2.4.2. Betaine
2.4.3. Sugars
2.4.4. γ-Aminobutyric Acid (GABA)
2.4.5. Succinic, Acetic, and Fumaric Acids
2.4.6. Methanol
2.5. Influence of Drying Methods on the Metabolic Composition of H. sabdariffa Calyces
2.6. Influence of Sample Location on the Metabolic Composition of H. sabdariffa Calyces
3. Materials and Methods
3.1. Reagents
3.2. Plant Materials
3.3. Drying Process
3.3.1. Shade Drying (SD)
3.3.2. Tray Drying (TD)
3.4. Proximate Analysis
3.4.1. Moisture
3.4.2. Ash Content
3.4.3. Crude Fiber
3.4.4. Crude Protein
3.4.5. Total Lipid Content
3.5. Extraction of Metabolites for NMR Analysis
3.6. NMR Sample Preparation
3.7. NMR Data Acquisition and Processing
3.8. Metabolite Quantification
3.9. Statistical Data Analysis
3.9.1. Principal Component Analysis (PCA)
3.9.2. Bivariate Correlation Analysis
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Sample Availability
References
- Tilburt, J.C.; Kaptchuk, T.J. Herbal medicine research and global health: An ethical analysis. Bull. World Health Organ. 2008, 86, 594–599. [Google Scholar] [CrossRef]
- Goraya, G.S.; Ved, D.K. Medicinal Plants in India: An Assessment of Their Demand and Supply; NMPB, New Delhi & FRLHT: Bangalore, India, 2017. [Google Scholar]
- Agarwal, J.; Dedhia, E. Current Scenario of Hibiscus sabdariffa (Mesta) in India. Int. J. Soc. Sci. Humanit. Invent. 2014, 1, 129–135. [Google Scholar]
- Plotto, A. Hibiscus–Post Production Management for Improved Market Access. In INPhP–Post–harvest Compendium; Mazaud, F., Rottger, A., Steffel, K., Eds.; FAO: Rome, Italy, 2004. [Google Scholar]
- Jabeur, I.; Pereira, E.; Barros, L.; Calhelha, R.C.; Sokovic, M.; Oliveira, M.B.P.; Ferreira, I.C. Hibiscus sabdariffa L. as a sourse of nutrients, bioactive compounds and colouring agent. Food Res. Int. 2017, 100, 717–723. [Google Scholar] [CrossRef] [Green Version]
- Da-Costa-Rocha, I.; Bonnlaender, B.; Sievers, H.; Pischel, I.; Heinrich, M. Hibiscus sabdariffa L.–A phytochemical and pharmacological review. J. Food Chem. 2014, 165, 424–443. [Google Scholar] [CrossRef] [Green Version]
- Montes-Rubio, P.Y.; Fabela-Illescas, H.E. Bioactive Compounds and Antihypertensive Activity of Extracts of Hibiscus sabdariffa L. Mex. J. Med Res. ICSA 2019, 7, 12–18. [Google Scholar] [CrossRef]
- Abubakar, M.; Ukwuani, A.; Mande, U. Antihypertensive activity of Hibiscus sabdariffa aqueous calyx extract in Albino rats. Sky J. Biochem. Res. 2015, 4, 16–20. [Google Scholar]
- Onyenekwe, P.C.; Ajani, E.O.; Ameh, D.A.; Gamaniel, K.S. Antihypertensive effect of roselle (Hibiscus sabdariffa) calyx infusion in spontaneously hypertensive rats and a comparison of its toxicity with that in Wistar rats Cell. Biochem. Funct. 1999, 17, 199–206. [Google Scholar] [CrossRef]
- Diez-Echave, P.; Vezza, T.; Rodríguez-Nogales, A.; Ruiz-Malagón, A.J.; Hidalgo-García, L.; Garrido-Mesa, J.; Molina-Tijeras, J.A.; Romero, M.; Robles-Vera, I.; Pimentel-Moral, S.; et al. The prebiotic properties of Hibiscus sabdariffa extract contribute to the beneficial effects in diet-induced obesity in mice. Food Res. Int. 2020, 127, 108722. [Google Scholar] [CrossRef] [PubMed]
- Jabeur, I.; Pereira, E.; Caleja, C.; Calhelha, R.C.; Soković, M.; Catarino, L.; Barros, L.; Ferreira, I.C. Exploring the chemical and bioactive properties of Hibiscus sabdariffa L. calyces from Guinea-Bissau (West Africa). Food Funct. 2019, 10, 2234–2243. [Google Scholar] [CrossRef] [PubMed] [Green Version]
- Ojulari, O.V.; Lee, S.G.; Nam, J.O. Beneficial Effects of Natural Bioactive Compounds from Hibiscus sabdariffa L. on Obesity. Molecules 2019, 24, 210. [Google Scholar] [CrossRef] [Green Version]
- Joachim, M.; Albert, H. Drying of Medicinal Plants. In Medicinal and Aromatic Plants-Agricultural, Commercial, Ecological, Legal, Pharmacological and Social Aspects; Bogers, R.J., Craker, L.E., Lange, D., Eds.; Springer: Berlin/Heidelberg, Germany, 2006; pp. 237–252. [Google Scholar]
- Tham, T.C.; Ng, M.X.; Gan, S.H.; Chua, L.S.; Aziz, R.; Abdullah, L.C.; Law, C.L. Impacts of different drying strategies on drying characteristics, the retention of bio-active ingredient and colour changes of dried Roselle. Chin. J. Chem. Eng. 2018, 26, 303–316. [Google Scholar] [CrossRef]
- Kim, H.K.; Choi, Y.H.; Verpoorte, R. NMR-based metabolomic analysis of plants. Nat. Protoc. 2010, 5, 536–549. [Google Scholar] [CrossRef]
- Ebbels, T.M.; Cavill, R. Bioinformatic methods in NMR-based metabolic profiling. Prog. Nucl. Magn. Reson. Spectrosc. 2009, 55, 361–374. [Google Scholar] [CrossRef]
- Hachem, R.; Assemat, G.; Martins, N.; Balayssac, S.; Gilard, V.; Martino, R.; Malet-Martino, M. Proton NMR for detection, identification and quantification of adulterants in 160 herbal food supplements marketed for weight loss. J. Pharm. Biomed. Anal. 2016, 124, 34–47. [Google Scholar] [CrossRef] [PubMed]
- Monakhova, Y.B.; Kuballa, T.; Löbell-Behrends, S.; Hengen, J.; Maixner, S.; Kohl-Himmelseher, M.; Lachenmeier, D.W. 1H NMR screening of pharmacologically active substances in weight-loss supplements being sold online. Lebensmittelchemie 2012, 66, 147–150. [Google Scholar] [CrossRef]
- Seethapathy, G.S.; Tadesse, M.; Urumarudappa, S.K.J.; Gunaga, S.V.; Vasudeva, R.; Malterud, K.E.; Shaanker, R.U.; de Boer, H.J.; Ravikanth, G.A.; Wangensteen, H. Authentication of Garcinia fruits and food supplements using DNA barcoding and NMR spectroscopy. Sci. Rep. 2018, 8, 10561. [Google Scholar] [CrossRef]
- Maciel, L.G.; do Carmo, M.A.V.; Azevedo, L.; Daguer, H.; Molognoni, L.; de Almeida, M.M.; Rosso, N.D. Hibiscus sabdariffa anthocyanins-rich extract: Chemical stability in vitro antioxidant and antiproliferative activities. J. Fct. 2018, 113, 187–197. [Google Scholar] [CrossRef] [PubMed]
- Miranda-Medina, A.; Hayward-Jones, P.M.; Carvajal-Zarrabal, O.; de Guevara, L.D.A.L.; Ramírez-Villagómez, Y.D.; Barradas-Dermitz, D.M.; Aguilar-Uscanga, M.G. Optimization of Hibiscus sabdariffa L. (Roselle) anthocyanin aqueous-ethanol extraction parameters using response surface methodology. Sci. Study Res. Chem. Chem. Eng. Biotechnol. Food Ind. 2018, 19, 53–62. [Google Scholar]
- Pham, T.N.; Nguyen, T.N.P.; Lam, T.D.; Tran, T.H.; Nguyen, D.C.; Vo, D.V.N.; Bach, L.G. Effects of various solvent concentration, liquid-solid ratio, temperatures and time values on the extraction yield of anthocyanin from Vietnam Hibiscus sabdariffa L. (Roselle). In IOP Conference Series Materials Science and Engineering; IOP Publishing: Bristol, UK, 2019; p. 542. [Google Scholar]
- Sipahli, S.; Mohanlall, V.; Mellem, J.J. Stability and degradation kinetics of crude anthocyanin extracts from H. sabdariffa. Food Sci. Technol. 2017, 37, 209–215. [Google Scholar] [CrossRef] [Green Version]
- Wu, H.-Y.; Yang, K.-M.; Chiang, P.-Y. Roselle anthocyanins: Antioxidant properties and stability to heat and pH. Molecules 2018, 23, 1357. [Google Scholar] [CrossRef] [Green Version]
- Vega-Gálvez, A.; Zura-Bravo, L.; Lemus-Mondaca, R.; Martinez-Monzó, J.; Quispe-Fuentes, I.; Puente, L.; Di Scala, K. Influence of drying temperature on dietary fibre, rehydration properties, texture and microstructure of Cape gooseberry (Physalis peruviana L.). J. Food Sci. Technol. 2015, 52, 2304–2311. [Google Scholar] [CrossRef] [Green Version]
- Amoasah, B.; Appiah, F.; Kumah, P. Effects of different drying methods on proximate composition of three accessions of roselle (Hibiscus sabdariffa) Calyce. Int. J. Plant Soil Sci. 2018, 21, 1–8. [Google Scholar] [CrossRef]
- Zheoat, A.M.; Gray, A.I.; Igoli, J.O.; Kennedy, A.R.; Ferro, V.A. Crystal structures of hibiscus acid and hibiscus acid dimethyl ester isolated from Hibiscus sabdariffa (Malvaceae). Acta Crystallogr. Sect. E Crystallogr. Commun. 2017, 73, 1368–1371. [Google Scholar] [CrossRef] [PubMed] [Green Version]
- Adams, C.J.; Grainger, M.N.; Manley-Harris, M. Isolation of maltol glucoside from the floral nectar of New Zealand mānuka (Leptospermum scoparium). Food Chem. 2015, 174, 306–309. [Google Scholar] [CrossRef] [PubMed]
- Zheoat, A.M.; Gray, A.I.; Igoli, J.O.; Ferro, V.A.; Drummond, R.M. Hibiscus acid from Hibiscus sabdariffa (Malvaceae) has a vasorelaxant effect on the rat aorta. Fitoterapia 2019, 134, 5–13. [Google Scholar] [CrossRef] [PubMed] [Green Version]
- Craig, S.A.S. Betaine in human nutrition. Am. J. Clin. Nutr. 2004, 80, 539–549. [Google Scholar] [CrossRef] [Green Version]
- Lim, L.S.; Chor, W.K.; Tuzan, A.D.; Shapawi, R.; Kawamura, G. Betaine is a feed enhancer for juvenile grouper (Epinephelus fuscoguttatus) as determined behaviourally. J. Appl. Anim. Res. 2016, 44, 415–418. [Google Scholar] [CrossRef]
- Jayasinghe, S.N.; Kruger, R.; Walsh, D.C.; Cao, G.; Rivers, S.; Richter, M.; Breier, B.H. Is sweet taste perception associated with sweet food liking and intake? Nutrients 2017, 9, 750. [Google Scholar] [CrossRef] [PubMed] [Green Version]
- Low, J.Y.; McBride, R.L.; Lacy, K.E.; Keast, R.S. Psychophysical evaluation of sweetness functions across multiple sweeteners. Chem. Senses 2017, 42, 111–120. [Google Scholar] [CrossRef] [PubMed] [Green Version]
- Diana, M.; Quílez, J.; Rafecas, M. Gamma-aminobutyric acid as a bioactive compound in foods: A review. J. Funct. Foods 2014, 10, 407–420. [Google Scholar] [CrossRef]
- Okada, T.; Sugishita, T.; Murakami, T.; Murai, H.; Saikusa, T.; Horino, T.; Takahashi, T. Effect of the defatted rice germ enriched with GABA for sleeplessness, depression, autonomic disorder by oral administration. J. Jpn. Soc. Food Sci. Technol. 2000, 4, 596–603. [Google Scholar] [CrossRef] [Green Version]
- Pouliot-Mathieu, K.; Gardner-Fortier, C.; Lemieux, S.; St-Gelais, D.; Champagne, C.P.; Vuillemard, J.C. Effect of cheese containing gamma-aminobutyric acid-producing lactic acid bacteria on blood pressure in men. PharmaNutrition 2013, 1, 141–148. [Google Scholar] [CrossRef]
- Yoshimura, M.; Toyoshi, T.; Sano, A.; Izumi, T.; Fujii, T.; Konishi, C.; Obata, A. Antihypertensive effect of a γ-aminobutyric acid rich tomato cultivar ‘DG03-9’in spontaneously hypertensive rats. J. Agric. Food Chem. 2010, 58, 615–619. [Google Scholar] [CrossRef] [PubMed]
- Moon, C.S. Estimations of the lethal and exposure doses for representative methanol symptoms in humans. Ann. Occup. Environ. Med. 2017, 29, 44. [Google Scholar] [CrossRef] [PubMed]
- Possner, D.; Zimmer, T.; Kürbel, P.; Dietrich, H. Methanol contents of fruit juices and smoothies in comparison to fruits and a simple method for the determination thereof. Dtsch. Lebensm. Rundsch. 2014, 110, 65–69. [Google Scholar]
- Gänzle, M.G. Lactic metabolism revisited: Metabolism of lactic acid bacteria in food fermentations and food spoilage. Curr. Opin. Food Sci. 2015, 2, 106–117. [Google Scholar] [CrossRef]
- AOAC. Official Methods of Analysis of AOAC International; Association of Official Analytical Chemists: Washington, DC, USA, 1995. [Google Scholar]
- Bligh, E.G.; Dyer, W.J. A rapid method of total lipid extraction and purification. Can. J. Biochem. Physiol. 1959, 37, 911–917. [Google Scholar] [CrossRef] [Green Version]
- Shumilina, E.; Ciampa, A.; Capozzi, F.; Rustad, T.; Dikiy, A. NMR approach for monitoring post-mortem changes in Atlantic salmon fillets stored at 0 and 4 C. Food Chem. 2015, 184, 12–22. [Google Scholar] [CrossRef] [Green Version]
- Ulrich, E.L.; Akutsu, H.; Doreleijers, J.F.; Harano, Y.; Ioannidis, Y.E.; Lin, J.; Nakatani, E. BioMagResBank. Nucleic Acids Res. 2007, 36, D402–D408. [Google Scholar] [CrossRef] [PubMed] [Green Version]
- Wishart, D.S.; Tzur, D.; Knox, C.; Eisner, R.; Guo, A.C.; Young, N.; Fung, C. HMDB: The human metabolome database. Nucleic Acids Res. 2007, 35, D521–D526. [Google Scholar] [CrossRef] [PubMed]
Location | Moisture Content (%) | Ash Content (%) | Crude Fiber (%) | Crude Protein (%) | Lipid Content (%) | |||||
---|---|---|---|---|---|---|---|---|---|---|
SD | TD | SD | TD | SD | TD | SD | TD | SD | TD | |
1 | 9.10 ± 1.50 | 6.11 ± 0.19 | 4.88 ± 0.38 | 5.10 ± 0.38 | 6.29 ± 0.28 | 4.82 ± 0.31 | 8.33 ± 0.45 | 8.18 ± 0.60 | 2.32 ± 0.36 | 3.99 ± 0.55 |
2 | 5.93 ± 1.55 | 2.99 ± 0.52 | 5.16 ± 0.53 | 6.29 ± 0.05 | 11.87 ± 0.49 | 10.51 ± 0.10 | 8.21 ± 0.36 | 7.65 ± 0.17 | 3.33 ± 0.44 | 6.77 ± 1.08 |
3 | 8.34 ± 0.90 | 4.65 ± 0.66 | 4.50 ± 0.05 | 5.44 ± 0.87 | 16.38 ± 0.04 | 15.07 ± 0.04 | 7.73 ± 0.07 | 8.70 ± 0.58 | 4.79 ± 0.76 | 7.84 ± 1.09 |
4 | 7.57 ± 1.44 | 4.72 ± 0.77 | 4.60 ± 0.04 | 6.33 ± 0.40 | 19.53 ± 0.01 | 19.02 ± 0.20 | 7.88 ± 0.20 | 6.96 ± 0.48 | 4.57 ± 0.88 | 7.54 ± 0.01 |
5 | 14.0 ± 2.01 | 8.66 ± 0.57 | 4.36 ± 0.38 | 6.43 ± 0.40 | 17.65 ± 0.03 | 16.25 ± 0.03 | 8.24 ± 0.04 | 8.41 ± 0.71 | 2.19 ± 0.27 | 3.78 ± 0.21 |
6 | 9.10 ± 1.50 | 7.20 ± 1.09 | 4.33 ± 0.57 | 5.66 ± 0.57 | 18.65 ± 0.03 | 18.22 ± 0.01 | 8.12 ± 0.26 | 8.05 ± 0.65 | 3.20 ± 0.24 | 6.02 ± 0.76 |
7 | 12.74 ± 0.18 | 10.66 ± 0.11 | 4.43 ± 0.16 | 6.29 ± 0.25 | 19.04 ± 0.01 | 17.85 ± 0.03 | 8.49 ± 0.3 | 9.33 ± 0.79 | 3.57 ± 0.14 | 6.83 ± 0.31 |
8 | 15.13 ± 0.11 | 15.03 ± 0.16 | 4.77 ± 0.68 | 6.51 ± 0.48 | 16.56 ± 0.02 | 16.26 ± 0.05 | 8.00 ± 0.12 | 8.38 ± 0.61 | 2.94 ± 0.90 | 7.65 ± 0.04 |
9 | 7.97 ± 1.25 | 5.88 ± 1.18 | 4.07 ± 0.13 | 6.07 ± 0.07 | 19.18 ± 0.10 | 17.92 ± 0.04 | 8.60 ± 0.22 | 7.37 ± 0.35 | 3.96 ± 0.39 | 34.00 ± 0.23 |
10 | 12.29 ± 0.62 | 10.77 ± 0.73 | 4.36 ± 0.55 | 6.95 ± 0.07 | 15.76 ± 0.32 | 13.81 ± 0.12 | 8.00 ± 0.62 | 8.08 ± 0.37 | 3.51 ± 0.13 | 5.92 ± 0.16 |
11 | 11.24 ± 0.26 | 9.16 ± 0.88 | 4.13 ± 0.06 | 6.01 ± 0.02 | 18.64 ± 0.10 | 18.30 ± 0.20 | 8.05 ± 0.83 | 7.12 ± 0.08 | 2.20 ± 0.31 | 3.66 ± 0.22 |
12 | 10.17 ± 0.14 | 7.00 ± 0.11 | 4.45 ± 0.40 | 6.02 ± 0.13 | 16.44 ± 0.05 | 14.89 ± 0.10 | 7.77 ± 0.50 | 7.62 ± 0.63 | 4.95 ± 0.41 | 7.14 ± 0.41 |
13 | 15.23 ± 0.20 | 11.18 ± 0.23 | 4.24 ± 0.04 | 6.02 ± 0.04 | 17.02 ± 0.05 | 15.92 ± 0.05 | 8.49 ± 0.17 | 9.09 ± 0.23 | 3.52 ± 0.08 | 5.94 ± 0.28 |
14 | 12.50 ± 0.48 | 10.45 ± 0.30 | 4.16 ± 0.15 | 6.65 ± 0.09 | 15.50 ± 0.07 | 13.32 ± 0.08 | 7.04 ± 0.08 | 5.66 ± 0.66 | 3.63 ± 0.13 | 5.38 ± 0.21 |
15 | 8.44 ± 0.73 | 6.03 ± 0.83 | 4.33 ± 0.57 | 5.99 ± 0.01 | 18.73 ± 0.13 | 17.76 ± 0.19 | 6.73 ± 0.10 | 5.52 ± 0.10 | 2.11 ± 0.26 | 4.04 ± 0.54 |
16 | 7.77 ± 0.39 | 6.01 ± 0.29 | 4.33 ± 0.57 | 5.66 ± 0.57 | 19.44 ± 0.27 | 16.90 ± 0.03 | 7.77 ± 0.56 | 7.93 ± 0.04 | 2.69 ± 0.77 | 5.55 ± 0.38 |
Average | 10.47 ± 0.83 | 7.91 ± 0.54 | 4.44 ± 0.33 | 6.09 ± 0.28 | 16.67 ± 0.13 | 15.43 ± 0.10 | 7.96 ± 0.31 | 7.75 ± 0.44 | . 3.34 ± 0.41 | 5.75 ± 0.41 |
N | δ. ppm | Mult. | J | HSQC | Assign. | Compound |
---|---|---|---|---|---|---|
1 | 0.99 | d | 7.00 | 19.9 | CH3 | Valine |
2 | 1.02 | d | 6.90 | 17.1 | CH3 | Isoleucine |
1 | 1.04 | d | 7.00 | 20.2 | CH3 | Valine |
3 | 1.19 | t | 7.10 | 19.5 | CH3 | Ethanol |
4 | 1.48 | d | 7.13 | 19.1 | CH3 | Alanine |
5 | 1.89 | m | 26.5 | CH2 | GABA # | |
6 | 1.93 | s | 26 | CH3 | Acetate | |
7 | 1.99 | m | 26.5 | CH2 | Proline | |
7 | 2.06 | m | 31.6 | CH | Proline | |
5 | 2.3 | t | 7.38 | 37.3 | CH2 | GABA |
7 | 2.34 | m | 31.7 | CH | Proline | |
8 | 2.41 | s | 37 | 2(CH2) | Succinate | |
9 | 2.46 | t | 6.87 | CH2 | 2-oxoglutarate * | |
10 | 2.77 | d | 17.86 | 44.9 | CH | Hibiscus acid |
11 | 2.86 | m | 8.30 | 37.6 | CH | Asparagine |
11 | 2.96 | m | 8.30 | 37.6 | CH | Asparagine |
9 | 3.01 | t | 6.87 | CH2 | 2-oxoglutarate * | |
5 | 3.02 | t | 7.50 | 42.3 | CH2 | GABA |
10 | 3.21 | d | 17.86 | 44.9 | CH | Hibiscus acid |
12 | 3.25 | m | 77.2 | CH | Glucose | |
13 | 3.27 | s | 56.2 | 3(CH3) | Betaine | |
14 | 3.35 | s | 76.5 | Scyllo-inositol | ||
15 | 3.37 | s | 51.9 | CH3 | Methanol | |
12 | 3.38–3.86 | Sugars | ||||
12 | 3.89 | m | CH | Glucose | ||
13 | 3.9 | s | 69.2 | CH2 | Betaine | |
16 | 3.99–4.04 | m | Fructose | |||
16 | 4.12 | d | 3.71 | 78 | Fructose | |
17 | 4.52 | d | 7.78 | 99.8 | CH | Arabinose |
12 | 4.64 | d | 98.9 | CH | Glucose | |
10 | 5.17 | s | 87.9 | CH | Hibiscus acid | |
12 | 5.24 | d | 95.2 | CH | Glucose | |
17 | 5.25 | d | overlap | Arabinose | ||
18 | 6.5–6.37 | m | 117.3–117.6 | Maltol * | ||
19 | 6.52 | s | 138.3 | Fumaric acid | ||
18 | 7.75–7.62 | m | 149 | Maltol * | ||
20 | 8.45 | s | Formic acid |
2.3 | 6.44 | 6.46 | 6.52 | 7.23 | 7.65 | 7.66 | 7.68 | 7.69 | |
2.30 | 0.97 | 0.98 | 0.92 | 0.98 | 0.97 | 0.94 | 0.96 | 0.96 | |
6.44 | 0.97 | 1.00 | 0.92 | 0.99 | 0.98 | 0.97 | 0.98 | 0.98 | |
6.46 | 0.98 | 1.00 | 0.90 | 0.99 | 0.98 | 0.95 | 0.97 | 0.97 | |
6.52 | 0.92 | 0.92 | 0.90 | 0.90 | 0.90 | 0.89 | 0.90 | 0.89 | |
7.23 | 0.98 | 0.99 | 0.99 | 0.90 | 0.99 | 0.96 | 0.98 | 0.98 | |
7.65 | 0.97 | 0.98 | 0.98 | 0.90 | 0.99 | 0.96 | 0.98 | 0.98 | |
7.66 | 0.94 | 0.97 | 0.95 | 0.89 | 0.96 | 0.96 | 0.99 | 0.99 | |
7.68 | 0.96 | 0.98 | 0.97 | 0.90 | 0.98 | 0.98 | 0.99 | 0.99 | |
7.69 | 0.96 | 0.98 | 0.97 | 0.89 | 0.98 | 0.98 | 0.99 | 0.99 |
Sample No. | Hibiscus acid | Betaine | Glucose | Fructose | GABA | Succinate | Acetate | Fumarate | Alanine | Methanol |
---|---|---|---|---|---|---|---|---|---|---|
S1 | 12,421 ± 82 | 225.7 ± 1.5 | 1639 ± 13 | 1609 ± 7 | 111.3 ± 5.3 | 131.6 ± 5.1 | 169 ± 2 | 39.59 ± 1.04 | 20.17 ± 0.00 | 30.47 ± 0.09 |
T1 | 13,119 ± 65 | 279.8 ± 0.3 | 2080 ± 5 | 1971 ± 10 | 57.7 ± 0.9 | 134.7 ± 3.1 | 147 ± 3 | 24.03 ± 0.33 | 15.19 ± 0.08 | 12.50 ± 0.03 |
S2 | 11,479 ± 57 | 219.2 ± 2.1 | 1662 ± 7 | 1652 ± 0 | 92.0 ± 4.0 | 131.7 ± 2.0 | 175 ± 0 | 37.35 ± 1.70 | 19.94 ± 0.18 | 39.79 ± 0.12 |
T2 | 12,411 ± 51 | 298.2 ± 4.1 | 2418 ± 9 ± | 2115 ± 14 | 61.7 ± 1.7 | 166.4 ± 2.1 | 161 ± 1 | 22.47 ± 0.57 | 16.84 ± 0.08 | 33.63 ± 0.23 |
S3 | 12,621 ± 87 | 225.5 ± 0.4 | 1578 ± 5 | 1594 ± 2 | 97.0 ± 3.9 | 128.3 ± 1.5 | 162 ± 2 | 40.04 ± 0.40 | 19.47 ± 0.12 | 24.72 ± 0.10 |
T3 | 14,452 ± 67 | 316.6 ± 0.6 | 2508 ± 1 | 2179 ± 5 | 65.8 ± 3.3 | 146.8 ± 10.8 | 165 ± 0 | 25.01 ± 0.90 | 16.90 ± 0.00 | 18.10 ± 0.08 |
S4 | 11,508 ± 76 | 217.0 ± 1.0 | 1645 ± 4 | 1649 ± 3 | 86.4 ± 3.2 | 128.7 ± 5.2 | 172 ± 1 | 31.89 ± 0.88 | 18.62 ± 0.27 | 35.96 ± 0.06 |
T4 | 14,011 ± 38 | 305.4 ± 0.6 | 2218 ± 5 | 2193 ± 5 | 57.4 ± 5.0 | 174.7 ± 7.7 | 164 ± 1 | 25.61 ± 1.13 | 16.89 ± 0.16 | 17.01 ± 0.25 |
S5 | 12,070 ± 95 | 220.3 ± 0.9 | 1609 ± 3 | 1623 ± 7 | 93.1 ± 3.2 | 126.7 ± 3.3 | 171 ± 1 | 38.79 ± 0.40 | 19.36 ± 0.20 | 33.30 ± 0.00 |
T5 | 13,975 ± 15 | 304.5 ± 1.0 | 2438 ± 5 | 2137 ± 2 | 58.7 ± 2.9 | 171.5 ± 2.5 | 170 ± 0 | 23.90 ± 0.86 | 16.75 ± 0.25 | 14.49 ± 0.12 |
S6 | 12,896 ± 88 | 231.4 ± 0.0 | 1590 ± 5 | 1521 ± 8 | 102.1 ± 0.2 | 114.7 ± 7.1 | 166 ± 1 | 41.29 ± 0.88 | 20.63 ± 0.33 | 21.99 ± 0.16 |
T6 | 14,537 ± 17 | 316.9 ± 0.2 | 2322 ± 5 | 2346 ± 5 | 62.1 ± 0.7 | 186.6 ± 2.6 | 172 ± 0 | 25.98 ± 1.19 | 17.94 ± 0.25 | 21.63 ± 0.21 |
S7 | 11,654 ± 88 | 208.6 ± 2.2 | 1604 ± 1 | 1568 ± 13 | 90.9 ± 0.8 | 114.7 ± 2.2 | 169 ± 1 | 31.73 ± 0.72 | 18.22 ± 0.16 | 34.64 ± 0.19 |
T7 | 14,435 ± 64 | 276.7 ± 3.0 | 2162 ± 6 | 2172 ± 4 | 57.6 ± 3.6 | 156.3 ± 5.7 | 142 ± 0 | 21.11 ± 1.63 | 14.76 ± 0.25 | 14.93 ± 0.51 |
S8 | 10,910 ± 29 | 194.6 ± 0.7 | 1567 ± 0 | 1513 ± 0 | 77.8 ± 1.2 | 103.5 ± 5.0 | 152 ± 0 | 20.55 ± 0.24 | 16.42 ± 0.00 | 12.12 ± 0.87 |
T8 | 14,898 ± 53 | 327.4 ± 0.4 | 2459 ± 3 | 2270 ± 9 | 63.5 ± 1.9 | 160.7 ± 6.4 | 167 ± 1 | 24.41 ± 0.48 | 17.67 ± 0.25 | 15.79 ± 0.09 |
S9 | 11,976 ± 89 | 207.9 ± 1.3 | 1581 ± 3 | 1551 ± 1 | 92.2 ± 2.3 | 119.1 ± 5.4 | 164 ± 0 | 34.37 ± 0.32 | 18.11 ± 0.25 | 24.03 ± 0.27 |
T9 | 13,376 ± 107 | 292.7 ± 3.8 | 2358 ± 0 | 2151 ± 0 | 59.4 ± 0.8 | 172.3 ± 12.6 | 162 ± 0 | 23.82 ± 1.14 | 16.72 ± 0.16 | 21.41 ± 0.25 |
S10 | 9811 ± 95 | 188.6 ± 1.7 | 1512 ± 4 | 1500 ± 16 | 76.7 ± 3.7 | 116.1 ± 2.2 | 167 ± 2 | 21.29 ± 0.16 | 16.19 ± 0.33 | 42.41 ± 0.13 |
T10 | 14,606 ± 10 | 323.1 ± 1.2 | 2539 ± 3 | 2272 ± 1 | 65.4 ± 3.3 | 176.1 ± 19.1 | 169 ± 0 | 24.59 ± 0.46 | 17.76 ± 0.25 | 19.64 ± 0.09 |
S11 | 12,136 ± 5 | 219.9 ± 1.5 | 1630 ± 0 | 1597 ± 2 | 96.4 ± 2.2 | 132.1 ± 7.0 | 170 ± 1 | 38.89 ± 1.62 | 19.84 ± 0.08 | 30.67 ± 0.12 |
T11 | 13,327 ± 40 | 301.1 ± 2.1 | 2405 ± 5 | 2129 ± 2 | 59.0 ± 0.4 | 170.4 ± 11.9 | 156 ± 1 | 24.85 ± 0.24 | 16.76 ± 0.16 | 23.23 ± 0.44 |
S12 | 12,641 ± 19 | 220.1 ± 2.2 | 1664 ± 3 | 1636 ± 4 | 99.5 ± 0.5 | 117.6 ± 1.8 | 170 ± 1 | 38.85 ± 0.60 | 19.78 ± 0.25 | 23.80 ± 0.05 |
T12 | 13,888 ± 61 | 307.0 ± 0.4 | 2407 ± 3 | 2104 ± 3 | 57.3 ± 2.1 | 143.4 ± 9.7 | 161 ± 1 | 24.08 ± 0.24 | 16.39 ± 0.00 | 18.13 ± 0.01 |
S13 | 12,555 ± 38 | 302.6 ± 0.7 | 2190 ± 0 | 2018 ± 1 | 48.0 ± 2.3 | 163.4 ± 2.5 | 116 ± 1 | 22.41 ± 0.65 | 14.84 ± 0.08 | 16.41 ± 0.12 |
T13 | 13,376 ± 84 | 288.1 ± 1.8 | 2408 ± 3 | 2120 ± 1 | 56.1 ± 0.8 | 145.0 ± 8.5 | 158 ± 0 | 22.88 ± 0.78 | 16.38 ± 0.00 | 21.83 ± 0.03 |
S14 | 13,244 ± 58 | 314.8 ± 0.8 | 2301 ± 10 | 2100 ± 21 | 52.8 ± 2.4 | 164.0 ± 11.0 | 111 ± 0 | 23.85 ± 0.56 | 14.97 ± 0.25 | 15.31 ± 0.24 |
T14 | 15,119 ± 36 | 337.3 ± 2.7 | 2684 ± 4 | 2346 ± 2 | 63.9 ± 1.7 | 165.1 ± 12.9 | 180 ± 2 | 26.69 ± 0.31 | 18.20 ± 0.17 | 23.77 ± 0.09 |
S15 | 12,226 ± 54 | 303.3 ± 2.7 | 2121 ± 4 | 1953 ± 4 | 46.5 ± 1.2 | 178.0 ± 1.9 | 131 ± 0 | 23.16 ± 0.41 | 14.23 ± 0.17 | 21.86 ± 0.00 |
T15 | 15,502 ± 48 | 344 ± 1.3 | 2742 ± 1 | 2407 ± 4 | 64.5 ± 1.4 | 167.7 ± 10.8 | 183 ± 0 | 27.54 ± 0.26 | 18.57 ± 0.16 | 29.47 ± 0.32 |
S16 | 11,370 ± 72 | 301.3 ± 1.0 | 2018 ± 9 | 1902 ± 2 | 43.7 ± 1.6 | 195.2 ± 4.5 | 145 ± 1 | 24.69 ± 0.64 | 13.21 ± 0.00 | 23.65 ± 0.01 |
T16 | 14,544 ± 26 | 323.4 ± 1.8 | 2519 ± 18 | 2242 ± 2 | 59.1 ± 0.2 | 171.2 ± 10.4 | 170 ± 0 | 25.02 ± 0.18 | 17.53 ± 0.17 | 20.15 ± 0.00 |
St.Dev. SD (%) | 7.1 | 17.7 | 14.6 | 11.4 | 26.8 | 19.1 | 13 | 24.6 | 13.6 | 32.7 |
St.Dev. TD (%) | 5.8 | 6.3 | 7.1 | 5.1 | 5.3 | 8.7 | 6.4 | 6.5 | 6 | 27 |
Sample | District | Topography | Location | Harvesting Time |
---|---|---|---|---|
1 | Noida, Uttar Pradesh | 28.5439° N, 77.3333° E | Amity University | November |
2 | North, Meghalaya | 25.8987° N, 90.6019° E | Kharkutta | |
3 | Resubelpara | |||
4 | East, Meghalaya | 25.5672° N, 90.5258° E | Songsak | |
5 | Williamnagar | |||
6 | Rongjeng | |||
7 | West, Meghalaya | 25.5679° N, 90.2245° E | Betasing | December |
8 | Dalu | |||
9 | Selsella | |||
10 | Dadengiri | |||
11 | Tikirkilla | |||
12 | Tura | |||
13 | Zikzak | |||
14 | Chokpot | |||
15 | South, Meghalaya | 23.3301° N, 90.5636° E | Baghmara | |
16 | Rongara |
Experiment | Pulse Program | d1(S) | NS | RG | SW (ppm) | O1 (Hz) |
---|---|---|---|---|---|---|
1H | noesygppr1d | 4 | 128 | 57 | 20 | 2820 |
JRES | Jresgpprqf | 2 | 16/40 | 57 | 20 | 2820 |
1H-1H TOCSY | Mlevgpphprzf | 2 | 48 | 57 | 20 | 2820/2820 |
1H-13C HSQC | hsqcetgpprsisp2.2 | 2 | 48/128 | 203 | 20/165 | 2820/11,319 |
1H-13C HMBC | Hmbcgplpndprqf | 2 | 56/128 | 203 | 20/260 | 2820/18,110 |
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Marak, S.; Shumilina, E.; Kaushik, N.; Falch, E.; Dikiy, A. Effect of Different Drying Methods on the Nutritional Value of Hibiscus sabdariffa Calyces as Revealed by NMR Metabolomics. Molecules 2021, 26, 1675. https://doi.org/10.3390/molecules26061675
Marak S, Shumilina E, Kaushik N, Falch E, Dikiy A. Effect of Different Drying Methods on the Nutritional Value of Hibiscus sabdariffa Calyces as Revealed by NMR Metabolomics. Molecules. 2021; 26(6):1675. https://doi.org/10.3390/molecules26061675
Chicago/Turabian StyleMarak, Sengnolotha, Elena Shumilina, Nutan Kaushik, Eva Falch, and Alexander Dikiy. 2021. "Effect of Different Drying Methods on the Nutritional Value of Hibiscus sabdariffa Calyces as Revealed by NMR Metabolomics" Molecules 26, no. 6: 1675. https://doi.org/10.3390/molecules26061675