Alternating isocratic and step gradient elution high-speed counter-current chromatography for the isolation of minor phenolics from Ormocarpum kirkii bark

Kamto, Eutrophe Le Doux; Carvalho, Tatiane S. C.; Mbing, Joséphine Ngo; Matene, Marie C.N.; Pegnyemb, Dieudonné Emmanuel; Leitão, Gilda Guimarães

doi:10.1016/j.chroma.2016.12.026

Cited by 18 publications

(11 citation statements)

References 14 publications

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“…Off‐line comprehensive HSCCC×HPLC makes full use of the orthogonality of HSCCC and HPLC, preparative isolation of HSCCC, and high resolution of HPLC, which has great potential in complex natural products analysis [18–20]. HSCCC solvent systems (e.g., petroleum ether–ethyl acetate–methanol–water and ethyl acetate– n ‐butanol–water by simply adjusting volume ratios) have been widely used in purification of components with a broad range of polarities [18].…”

Section: Resultsmentioning

confidence: 99%

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Homoisoflavonoids profiling of Ophiopogon japonicus by off‐line coupling high‐speed countercurrent chromatography with high‐performance liquid chromatography–diode array detector‒quadrupole time‐of‐flight tandem mass spectrometry

Deng

Tong

et al. 2020

J of Separation Science

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Roots of Ophiopogon japonicus have been used as a functional food ingredient and traditional Chinese medicine for a long time in China. Homoisoflavonoids are one of the major kinds of bioactive compounds in O. japonicus; however, literature data about its homoisoflavonoids profile are scarce because of the complex ingredients with low abundance. Here, homoisoflavonoid fraction was prepared by petroleum ether extraction. Then, a high-speed countercurrent chromatography offline coupling with high-performance liquid chromatography-diode array detectorquadrupole time-of-flight tandem mass spectrometry was developed for systematic identification of homoisoflavonoids. After that, 39 homoisoflavonoids, including 29 homoisoflavanone and 10 homoisoflavone, were unambiguously or tentatively identified, while 12 of them were reported in O. japonicus for the first time. Finally, eight available homoisoflavonoids were sensitively, precisely, and accurately determined by standard calibration curves, with limit of detection and limit of quantification in the range of 0.05-0.30 μg/mL and 0.12-0.66 μg/mL, relative standard deviation less than 7.3% for intra-and interday variations, and recovery at 94.5-105.2%. Collectively, our developed method is efficient, reliable, and valuable to profile chemical components of complex natural products.

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Section: Resultsmentioning

confidence: 99%

“…Kemota et al. enriched 14 phenolics from Ormocarpum kirkii bark by HSCCC×HPLC and three new compounds were identified [20].…”

Section: Introductionmentioning

confidence: 99%

Homoisoflavonoids profiling of Ophiopogon japonicus by off‐line coupling high‐speed countercurrent chromatography with high‐performance liquid chromatography–diode array detector‒quadrupole time‐of‐flight tandem mass spectrometry

Deng

Tong

et al. 2020

J of Separation Science

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“…The revolution speed also has an impact on solid phase retention. Higher revolution speed would increase solid phase retention and shorten analysis process, but it may cause emulsification . Therefore, a rotary speed of 900 rpm was utilized.…”

Section: Resultsmentioning

confidence: 99%

Screening and separation of α‐amylase inhibitors from Solanum nigrum with amylase‐functionalized magnetic graphene oxide combined with high‐speed counter‐current chromatography

Cen

Xiao

Chen

et al. 2017

J of Separation Science

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A screening method using α-amylase-functionalized magnetic graphene oxide combined with high-speed counter-current chromatography was proposed and utilized to screen and separate α-amylase inhibitors from extract of Solanum nigrum. The α-amylase-functionalized magnetic graphene oxide was characterized and found to demonstrate satisfactory structure, magnetic response (24.5 emu/g), and reusability (retained 90% of initial activity after five cycles). The conditions for the screening with α-amylase functionalized magnetic graphene oxide were optimized and set at pH 7.0 and 25°C. As a result, two potent flavonoid compounds, apigenin-7-O-glucuronide (1) and astragalin (2), were separated and collected through high-speed counter-current chromatography and subjected to high-performance liquid chromatography analysis with purity higher than 90% (according to HPLC data), which were identified as α-amylase inhibitors. These results suggested that utilization of α-amylase functionalized magnetic graphene oxide in the rapid screening and isolation bioactive compounds from complex natural products is a feasible and environmentally friendly method.

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“…Thus, HSCCC has been widely used for the separation and purification of active components from natural products, albeit, it is a big challenge to separate all target components directly from crude extract in a single run. Therefore, the stepwise elution mode was introduced into HSCCC separation to address this problem . The common gradient modes used in counter‐current chromatography (CCC) include temperature gradients, stepwise flow‐rate gradients, stepwise solvent gradients, pH‐gradients, and salting‐out gradients.…”

Section: Introductionmentioning

confidence: 99%

“…Therefore, the stepwise elution mode was introduced into HSCCC separation to address this problem. [18][19][20] The common gradient modes used in counter-current chromatography (CCC) include temperature gradients, stepwise flow-rate gradients, 21,22 stepwise solvent gradients, 20,23 pH-gradients, and salting-out gradients. However, few articles related to HSCCC separation of natural products reported the combination of these gradient modes.…”

Section: Introductionmentioning

confidence: 99%

Separation of α‐glucosidase inhibitors from Potentilla kleiniana Wight et Arn using solvent and flow‐rate gradient high‐speed counter‐current chromatography target‐guided by ultrafiltration HPLC‐MS screening

Liu

Huang

Liu

et al. 2019

Phytochemical Analysis

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Introduction Potentilla kleiniana Wight et Arn is widely used as a herbal medicine to treat type 2 diabetes. However, detailed information about its active compounds is lacking. Objective To develop an efficient method for the rapid screening and separation of α‐glucosidase inhibitors from Potentilla kleiniana Wight et Arn. Methodology Potential α‐glucosidase inhibitors from Potentilla kleiniana Wight et Arn were rapidly screened out through ultrafiltration high‐performance liquid chromatography mass spectrometry (HPLC‐MS), and then followed by a target‐guided high‐speed counter‐current chromatography (HSCCC) separation using two‐phase solvent systems composed of n‐hexane/ethyl acetate/methanol/water (1:10:1:10, v/v/v/v and 1:10:5:6, v/v/v/v), and adopting increasing flow‐rate from 1.5 to 3.0 mL/min after 200 min. Their structures were identified by ultraviolet (UV), MS, proton nuclear magnetic resonance (1H‐NMR) and carbon‐13 (13C)‐NMR, and their α‐glucosidase inhibitory activities were assessed by in vitro assay. Results Five α‐glucosidase inhibitors including gallic acid (25.7 mg, 98.2%, 1), brevifolincarboxylic acid (9.86 mg, 95.3%, 2), ethyl evifolincarboxylate (13.26 mg, 97.6%, 3), 3,3′‐di‐O‐methylellagic acid‐4′‐O‐β‐d‐glucopyranoside (16.26 mg, 95.1%, 4), and 3,3′‐di‐O‐methylellagic acid (10.54 mg, 96.8%, 5) were successfully purified from 250 mg n‐butanol extract in a single run. Compounds 1, 2, 4 and 5 exhibited stronger α‐glucosidase inhibitory activities[half maximal inhibition concentration (IC50) values at 173.41 ± 6.35, 323.46 ± 8.08, 44.63 ± 2.50, and 20.73 ± 2.56 μM, respectively] than acarbose (IC50 value at 332.12 ± 5.52 μM, reference compound). Conclusions Notably, compounds 2–5 were reported in the Potentilla kleiniana Wight et Arn for the first time. The results indicated that the proposed method could be applied for the rapid screening and preparative separation of α‐glucosidase inhibitors from a complex matrix.

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Alternating isocratic and step gradient elution high-speed counter-current chromatography for the isolation of minor phenolics from Ormocarpum kirkii bark

Cited by 18 publications

References 14 publications

Homoisoflavonoids profiling of Ophiopogon japonicus by off‐line coupling high‐speed countercurrent chromatography with high‐performance liquid chromatography–diode array detector‒quadrupole time‐of‐flight tandem mass spectrometry

Homoisoflavonoids profiling of Ophiopogon japonicus by off‐line coupling high‐speed countercurrent chromatography with high‐performance liquid chromatography–diode array detector‒quadrupole time‐of‐flight tandem mass spectrometry

Screening and separation of α‐amylase inhibitors from Solanum nigrum with amylase‐functionalized magnetic graphene oxide combined with high‐speed counter‐current chromatography

Separation of α‐glucosidase inhibitors from Potentilla kleiniana Wight et Arn using solvent and flow‐rate gradient high‐speed counter‐current chromatography target‐guided by ultrafiltration HPLC‐MS screening

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