HPLC‒DAD‒QTOF-MS/MS based comprehensive metabolomic profiling of phenolic compounds in Kalimeris indica anti-inflammatory fractions

Xie, Lianwu; Lin, Qinlu; Guo, Keke; Tong, Chaoying; Shi, Shuyun; Shi, Feng

doi:10.1016/j.indcrop.2019.111636

Cited by 26 publications

(16 citation statements)

References 32 publications

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Section: Resultsmentioning

confidence: 99%

“…Flavonoids in natural products are important bioactive compounds and TFC have high positive correlations to their bioactive activities [12]. ZrOCl 2 colorimetric method contains high selectivity and accuracy by removal of the effect of phenolic acids with ortho‐hydroxy group [12]. As shown in Table 1, petroleum ether fraction yielded the highest TFC at 67.1 ± 3.0 μg QE/g DW, followed by ethyl acetate fraction at 5.9 ± 0.4 μg QE/g DW, water fraction at 2.8 ± 0.3 μg QE/g DW, and n ‐butanol fraction at 1.0 ± 0.1 μg QE/g DW.…”

Section: Resultsmentioning

confidence: 99%

“…ZrOCl 2 colorimetric method was selected to calculate TFC as our previously reported [12]. In brief, sample solution (2.0 mL, 3.0 mg/mL) was mixed with ZrOCl 2 solution (1.0 mL, 10.0 mg/mL), and then incubated at 30ºC for 1 h. After that, the absorbance was detected at 425 nm using an UV‐2600 spectrometer (Shimadzu, Tokyo, Japan).…”

Section: Methodsmentioning

confidence: 99%

“…HPLC with diode array detector (DAD) and MS/MS has been developed for rapid isolation and characterization of bioactive components from complex natural products [8–11]. However, information about comprehensive analysis of homoisoflavonoids, especially for minors, in O. japonicus by HPLC–DAD–MS/MS is restricted because of the existence of multicomponents, restriction of detection sensitivity, and coelution of minor and abundant compounds [12,13]. Therefore, techniques to enrich minors and improve separation resolutions are necessary for profiling homoisoflavonoids in O. japonicus .…”

Section: Introductionmentioning

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%

Section: Resultsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

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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“…The order of elution for caffeoyl quinic acid methyl ester was the same as reported in literature [ 24 ]. Alkyl ester of caffeoyl quinic acids are less common in natural products [ 25 ]. Thus, we can speculate that the above compounds are artifacts of methylation during acidic methanol extraction.…”

Section: Resultsmentioning

confidence: 99%

Simultaneous Qualitative and Quantitative Evaluation of the Coptidis Rhizoma and Euodiae Fructus Herbal Pair by Using UHPLC-ESI-QTOF-MS and UHPLC-DAD

Guo

et al. 2020

Molecules

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The herbal pair of Coptidis Rhizoma (CR) and Euodiae Fructus (EF) is a classical traditional Chinese medicine formula used for treating gastro-intestinal disorders. In this study, we established a systematic method for chemical profiling and quantification analysis of the major constituents in the CR-EF herbal pair. A method of ultra high performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UHPLC-QTOF-MS) for qualitative analysis was developed. Sixty-five compounds, including alkaloids, phenolics, and limonoids, were identified or tentatively assigned by comparison with reference standards or literature data. The UHPLC fingerprints of 19 batches of the CR-EF herbal pair samples were obtained and the reference fingerprint chromatograms were established. Furthermore, nine compounds among 24 common peaks of fingerprints were considered as marker components, which either had high contents or significant bioactivities, were applied to quality control of the CR-EF herbal pair by quantitative analysis. This UHPLC-DAD analysis method was validated by precision, linearity, repeatability, stability, recovery, and so on. The method was simple and sensitive, and thus reliable for quantitative and chemical fingerprint analysis for the quality evaluation and control of the CR-EF herbal pair and related traditional Chinese medicines.

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Diagnostic ion filtering targeted screening and isolation of anti‐inflammatory iridoid glycosides from Hedyotis diffusa

Shi

Tong

et al. 2021

J of Separation Science

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Efficient and targeted screening and isolation of bioactive compounds from complex natural products is still a challenging work. Herein, diagnostic ion filtering based high‐performance liquid chromatography–quadrupole time‐of‐flight−tandem mass spectrometry was firstly developed to screen six main iridoid glycosides from Hedyotis diffusa. Then, online extraction‒high‐speed counter current chromatography was proposed for targeted enrichment and preparative isolation using ethyl acetate/n‐butanol/water (4.5:0.5:5, v/v/v) as solvent system. After that, Sephadex LH‐20 column chromatography using methanol as solvent system was selected for further purification of six iridoid glycosides with purities over 98%. They were finally identified as monotropein, desacetylasperuloside acid, asperuloside, 6‐O‐(Z)‐p‐coumaroyl scandoside methyl ester, 6‐O‐(Z)‐feruloyl scandoside methyl ester, and 6‐O‐(E)‐p‐coumaroyl scandoside methyl ester. And their anti‐inflammatory activities were evaluated and confirmed by lipopolysaccharide activated RAW 264.7 macrophages. Obviously, the results provide a scientific basis for the potential applications of H. diffusa, and the developed methodology is efficient and reliable for targeted screening and isolation of bioactive compounds from natural products.

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HPLC‒DAD‒QTOF-MS/MS based comprehensive metabolomic profiling of phenolic compounds in Kalimeris indica anti-inflammatory fractions

Cited by 26 publications

References 32 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

Simultaneous Qualitative and Quantitative Evaluation of the Coptidis Rhizoma and Euodiae Fructus Herbal Pair by Using UHPLC-ESI-QTOF-MS and UHPLC-DAD

Diagnostic ion filtering targeted screening and isolation of anti‐inflammatory iridoid glycosides from Hedyotis diffusa

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