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Simultaneous Extraction Optimization and Analysis of Flavonoids from the Flowers of Tabernaemontana heyneana by High Performance Liquid Chromatography Coupled to Diode Array Detector and Electron Spray Ionization/Mass Spectrometry.

Sathishkumar T, Baskar R, Aravind M, Tilak S, Deepthi S, Bharathikumar VM - ISRN Biotechnol (2012)

Bottom Line: With the two different solvents, namely, ethanol and ethyl acetate, tried for the extraction optimization of flavonoid, ethanol (80.1 mg/g tissue) has been proved better than ethyl acetate (20.5 mg/g tissue).The optimal conditions of the extraction of flavonoid were found to be 85°C, 3 hours with a material ratio of 1 : 20, 75% ethanol, and 1 cycle of extraction.About seven different phenolics like robinin, quercetin, rutin, sinapoyl-hexoside, dicaffeic acid, and two unknown compounds were identified for the first time in the flowers of T. heyneana.

View Article: PubMed Central - PubMed

Affiliation: Department of Biotechnology, Kumaraguru College of Technology, Coimbatore 641049, India.

ABSTRACT
Flavonoids are exploited as antioxidants, antimicrobial, antithrombogenic, antiviral, and antihypercholesterolemic agents. Normally, conventional extraction techniques like soxhlet or shake flask methods provide low yield of flavonoids with structural loss, and thereby, these techniques may be considered as inefficient. In this regard, an attempt was made to optimize the flavonoid extraction using orthogonal design of experiment and subsequent structural elucidation by high-performance liquid chromatography-diode array detector-electron spray ionization/mass spectrometry (HPLC-DAD-ESI/MS) techniques. The shake flask method of flavonoid extraction was observed to provide a yield of 1.2 ± 0.13 (mg/g tissue). With the two different solvents, namely, ethanol and ethyl acetate, tried for the extraction optimization of flavonoid, ethanol (80.1 mg/g tissue) has been proved better than ethyl acetate (20.5 mg/g tissue). The optimal conditions of the extraction of flavonoid were found to be 85°C, 3 hours with a material ratio of 1 : 20, 75% ethanol, and 1 cycle of extraction. About seven different phenolics like robinin, quercetin, rutin, sinapoyl-hexoside, dicaffeic acid, and two unknown compounds were identified for the first time in the flowers of T. heyneana. The study has also concluded that L16 orthogonal design of experiment is an effective method for the extraction of flavonoid than the shake flask method.

No MeSH data available.


Related in: MedlinePlus

(a) Full scan ESI/MS spectra of parent ion of dicaffeic acid dimer at m/z 680 and fragment ions at m/z 340 (caffeic acid monomer), m/z 279, and m/z 184. (b) Parent ion of protonated form of kaempferol-3-O-robinoside-7-O-rhamnoside (robinin) at m/z 741 and [M + H]2−  m/z 740.
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fig6: (a) Full scan ESI/MS spectra of parent ion of dicaffeic acid dimer at m/z 680 and fragment ions at m/z 340 (caffeic acid monomer), m/z 279, and m/z 184. (b) Parent ion of protonated form of kaempferol-3-O-robinoside-7-O-rhamnoside (robinin) at m/z 741 and [M + H]2−  m/z 740.

Mentions: The MS spectra of peak B showed [M + H]2− at m/z 341, and fragment at m/z 184 (protonated form of caffeic acid) proved the presence of dicaffeic acid (dimer of caffeic acid). The fragmention at m/z 279 denoted the loss of acetate group. The MS spectra recorded at m/z 680 have proved the presence of dimer adduct of caffeic acid (Figure 6(a)). All the present investigation was well correlated with the results documented early [38]. Similarly, initial research work carried out by Sakushima et al. [39] by fast atom bombardment method has revealed the fragmentation mode of several flavonoid glycosides. From their studies, robinin was found to possess the parent ion at m/z 741 and the fragment ion m/z 433/287. In our present investigation, the parent ion as [M − H]+ was found as m/z 741, and the deprotonated form [M − H]− was m/z 740 (Figure 6(b)).


Simultaneous Extraction Optimization and Analysis of Flavonoids from the Flowers of Tabernaemontana heyneana by High Performance Liquid Chromatography Coupled to Diode Array Detector and Electron Spray Ionization/Mass Spectrometry.

Sathishkumar T, Baskar R, Aravind M, Tilak S, Deepthi S, Bharathikumar VM - ISRN Biotechnol (2012)

(a) Full scan ESI/MS spectra of parent ion of dicaffeic acid dimer at m/z 680 and fragment ions at m/z 340 (caffeic acid monomer), m/z 279, and m/z 184. (b) Parent ion of protonated form of kaempferol-3-O-robinoside-7-O-rhamnoside (robinin) at m/z 741 and [M + H]2−  m/z 740.
© Copyright Policy - open-access
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC4417552&req=5

fig6: (a) Full scan ESI/MS spectra of parent ion of dicaffeic acid dimer at m/z 680 and fragment ions at m/z 340 (caffeic acid monomer), m/z 279, and m/z 184. (b) Parent ion of protonated form of kaempferol-3-O-robinoside-7-O-rhamnoside (robinin) at m/z 741 and [M + H]2−  m/z 740.
Mentions: The MS spectra of peak B showed [M + H]2− at m/z 341, and fragment at m/z 184 (protonated form of caffeic acid) proved the presence of dicaffeic acid (dimer of caffeic acid). The fragmention at m/z 279 denoted the loss of acetate group. The MS spectra recorded at m/z 680 have proved the presence of dimer adduct of caffeic acid (Figure 6(a)). All the present investigation was well correlated with the results documented early [38]. Similarly, initial research work carried out by Sakushima et al. [39] by fast atom bombardment method has revealed the fragmentation mode of several flavonoid glycosides. From their studies, robinin was found to possess the parent ion at m/z 741 and the fragment ion m/z 433/287. In our present investigation, the parent ion as [M − H]+ was found as m/z 741, and the deprotonated form [M − H]− was m/z 740 (Figure 6(b)).

Bottom Line: With the two different solvents, namely, ethanol and ethyl acetate, tried for the extraction optimization of flavonoid, ethanol (80.1 mg/g tissue) has been proved better than ethyl acetate (20.5 mg/g tissue).The optimal conditions of the extraction of flavonoid were found to be 85°C, 3 hours with a material ratio of 1 : 20, 75% ethanol, and 1 cycle of extraction.About seven different phenolics like robinin, quercetin, rutin, sinapoyl-hexoside, dicaffeic acid, and two unknown compounds were identified for the first time in the flowers of T. heyneana.

View Article: PubMed Central - PubMed

Affiliation: Department of Biotechnology, Kumaraguru College of Technology, Coimbatore 641049, India.

ABSTRACT
Flavonoids are exploited as antioxidants, antimicrobial, antithrombogenic, antiviral, and antihypercholesterolemic agents. Normally, conventional extraction techniques like soxhlet or shake flask methods provide low yield of flavonoids with structural loss, and thereby, these techniques may be considered as inefficient. In this regard, an attempt was made to optimize the flavonoid extraction using orthogonal design of experiment and subsequent structural elucidation by high-performance liquid chromatography-diode array detector-electron spray ionization/mass spectrometry (HPLC-DAD-ESI/MS) techniques. The shake flask method of flavonoid extraction was observed to provide a yield of 1.2 ± 0.13 (mg/g tissue). With the two different solvents, namely, ethanol and ethyl acetate, tried for the extraction optimization of flavonoid, ethanol (80.1 mg/g tissue) has been proved better than ethyl acetate (20.5 mg/g tissue). The optimal conditions of the extraction of flavonoid were found to be 85°C, 3 hours with a material ratio of 1 : 20, 75% ethanol, and 1 cycle of extraction. About seven different phenolics like robinin, quercetin, rutin, sinapoyl-hexoside, dicaffeic acid, and two unknown compounds were identified for the first time in the flowers of T. heyneana. The study has also concluded that L16 orthogonal design of experiment is an effective method for the extraction of flavonoid than the shake flask method.

No MeSH data available.


Related in: MedlinePlus